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1、- - 4 JIS M*8124 79 I 4933b08 00bb379 9 JIS UDC 622.34 :543.062 : 546.47 , JAPANESE INDUSTRIAL STANDARD- Methods for Determination of Zinc in Ores JIS M 8 1 2 4 - 1 9 7 9 Translated and Published by Japanese Standards Association L Printed in Japan 9s Copyright Japanese Standards Association Provide
2、d by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*8L24 79 E 4933608 00bb3BO 5 In the event of any doubt arising, the original Standard in Japanese i
3、s to be final authority. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*8124 79 4933608 00bb38L 7
4、 E UDC 622.34:543.062:546.47 JAPANESE INDUSTRIAL STANDARD J I S MetQods for Determination of M 8124-1979 Zinc in Ores (Reaffirmed: 1984) 1. Scope This Japanese Industrial Standard specifies the methods for determination of zinc in ores. methods for determination of zinc are specified in other JIS. H
5、owever, this standard does not apply to the ores to which the 2. General Matters General matters common to the determination methods shall be as described in JIS K 0050 and JIS K 0121. 3. Sampling and Treating of Analysis Sample Sampling and Preparation of Sample 3.1 The sampling and preparation of
6、sample shall be as described in JIS M 8101 and JIS M 8083. 3.2 Weighing of Sample The weighing of a sample shall be as follows: (1) In weighing out a sample, thoroughly mix the sample bystirring carefully to represent average composition and further confirm no mixture with foreign matters, Put the s
7、ample into the air bath regulated at 105 k 5“C, dry it, take it out from the air bath at each 2 h and let it stand to cool in a desiccator to ordinary temperature. drying becomes not more than 0.1 % per 2 h. However, the drying conditions (temperature, time, etc.) of the sample liable to be deterior
8、ated because of containing sulfides or the like shall be as agreed between the parties concerned, (2) Repeat its drying until the loss on (3) For weighing out the sample, weigh out, as a rule, a specified amount to the nearest 1 mg by using a chemical balance. Applicable Standards: JIS K 0050-Genera
9、l Rules for Chemical Analysis JIS K 0121-General Rules for Atomic Absorption Spectrochemical Analysis JIS K 8005-Standard Substances for Volumetric Analysis JIS M 8083-Methods for Sampling of Non-Ferrous Flotation Concentrates in Bulk JIS M 8101-Methods for Sampling of Metal Bearing Ores of Copper,
10、JIS 2 8401-Rules for Rounding off of Nmerical Values Lead, Zinc, Tin, Gold, Silver and Others Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permi
11、tted without license from IHS -,-,- J I S Mu8124 79 E 4933608 00663B2 9 S 2 M 8124-1979 4. Expression of Analysis Value and Cautions on Operation 4.1 Expression of Analysis Value The expression of analysis value shall be as follows: (1) Express an analysis value in percentage and round off it to thr
12、ee places of decimals in accordance with JIS Z 8401. (2) Repeat the analysis two times in the same laboratory. difference between them is under the tolerance within the same laboratory, obtain their average and round off it to two places of decimals in accordance with JIS Z 8401 to be the report val
13、ue. When the (3) When the difference between analysis values obtained by repetition of two times exceeds the tolerance, carry out the analysis two times again. (4) The tolerance shall be as given in Table 1. Table 1. Tolerances ( l ) Unit: % Determination method Classification Within the same labora
14、tory (repetition) Ion-exchange separation 30 and over EDTA titrimetric method 10 to 30 excl. Precipitate separation 3 to 10 excl. 0.5 to 3 excl. EDTA titrimetric method 0.350 0.250 0.150 0.075 I i to 3 excl. I 0.3 to 1 excl. 0.1 to 0.3 excl. Atomic absorption method I 0.01 to 0.1 exci. I 0.150 0.040
15、 0.025 0.010 Note (I) When two analysis values extend over two classes, the tolerance of a class corresponding to average value of two analysis values shall be applied. 4.2 Cautions on Analytical Operation Cautions on analytical operation shall be as follows: (1) In analysis, a blank test shall be c
16、arried out through all the operation and the analysis value shall be corrected. (2) The flame of air and acetylene shall be used for the flame in atomic absorption method. However, if the conformance to the accuracy and precision has been confirmed, the flame of air and hydrogen and other flames may
17、 be used. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*8L24 79 O 4933608 00bb383 O O 3 M 8124-1
18、979 5. Determination Method 5.1 Classification of Methods The method for determination of zinc in ores shall be as described in either one of the following methods: ( 1) Ion-Exchange Separation EDTA Titrimetric Method This method shall (2) Precipitate Separation EDTA Titrimetric Method This method s
19、hall be applied to the sample of 0.5 % min. in zinc content. be applied to the sample of 0.5 % min. in zinc content (2). (3) Atomic Absorption Method This method shall be applied to the sample of 0.01 % and over to 3 % excl. in zinc content. Note ( 2 ) This method is applied to the sample which does
20、 not contain nickel and cobalt. 5.2 Ion-Exchange SeDaration EDTA Titrimetric Method 5.2.1 Purport After decomposing a sample with hydrochloric acid and nitric acid, and add sulfuric acid to generate white fume of sulfuric acid by heating. Dissolve soluble salts with water. After filtration, add hydr
21、ochloric acid and adsorb zinc by passing hydrochloric acid through an anion-exchange column. Then, remove copper, iron, etc. by passing dilute hydrochloric acid. Thereafter, elute zinc by passing ammonia-ammonium chloride. Add acetic acid and ammonium acetate thereto and regulate pH of the solution
22、at approx. 5.5. Thereafter, add ammonium fluoride and sodium thiosulfate, mask copper or the like, utilize Xylenol Orange as the indicator and titrate the sample solution with EDTA standard Reagents Hydrochloric acid Hydrochloric acid (1 t 5) Nitric acid Nitric acid (1 t 1) Hydrofluoric acid Hydrobr
23、omic acid The reagents shall be as follows: Sulfuric acid (1 t 1, 1 t 100) Aqueous ammonia Bromine Hydrochloric acid- ascorbic acid solution to 100 ml hydrochloric acid (1 + 5) to dissolve it. solution at each service. Ammonia-ammonium chloride solution to 1000 ml aqueous ammonia (7 t 100) to be dis
24、solved. Add 0.25 g ascorbic acid Prepare this Add 20 g ammonium chloride Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted without license
25、from IHS -,-,- J I S Mu8124 79 4933b08 00bb384 2 4 M 8124-1979 Ammonium fluoride solution (5 “Iv %) Sodium thiosulfate solution (pentahydrate) with water to 1000 ml. Dissolve 100 g sodium thiosulfate Acetic acid (1 t 1) Acetic acid-ammonium acetate mixed solution ammonium acetate with water to 1000
26、ml. acetic acid. Dissolve 250 g Thereafter, add 25 ml M/20 disodium ethylenediaminetetraacetate (EDTA) standard solution with water to 1000 ml. approx. 0.0033 g zinc, standardize it as follows: mg, decompose it with 10 ml hydrochloric acid (1 + 1) and add 180 ml ammonia-ammonium chloride solution. o
27、peration in accordance with the procedures of 5.2.5 (5) and (6) and obtain zinc equivalent amount per 1 ml EDTA standard solution from the following formula: Dissolve 18.6 g disodium ethylenediaminetetraacetate (dihydrate) Though 1 ml this solution corresponds to Weigh out 0.15 g zinc specified in J
28、IS K 8005 to the nearest 0.1 Thereafter, titrate it by where f : zinc equivalent amount of 1 ml EDTA standard solution (g) G: weighing out amount of zinc (g) v: use amount of EDTA standard solution (mi) M/ 1 O0 disodium ethylenediaminetetraacetate (EDTA) standard solution Dissolve 3.75 g disodium et
29、hylenediaminetetraacetate (dihydrate) with water to 1000 ml. Though 1 ml of this solution corresponds to approx. 0.00065 g zinc, accurately separately take 20 ml standard zinc solution and carry out its standardization in accordance with 5.2.2 (16), as appropriate. Standard zinc solution (1 mg Zn/ml
30、) specified in JIS K 8005 with 30 ml hydrochloric acid (1 t 2). cooling, transfer it into a measuring flask of 1000 ml and dilute it up to the marked line with water. Decompose 1.000 g zinc After Standard cadmium solution (20 pg Cd/ml) cadmium (99.9 % min.) with 20 ml nitric acid (1 t 1). After cool
31、ing, transfer it into a measuring flask of 1000 ml and dilute it up to the marked line with water. Accurately dilute a necessary amount 25 times at each service to be the standard cadmium solution. Decompose 0.500 g p-nitrophenol solution (0.1 “Iv %) Xylenol Orange (XO) solution (0.1 IV/“ %) Copyrig
32、ht Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS M*AL24 79 W 4933b08 00bb3B5 4 Under 30 30 and over 5 M 8124-1
33、979 0.5 to 1 0.25 to 0.5 5.2.3 Apparatus As a rule, the apparatus shall be as follows (3): As to an ion-exchange column, softly pack the absorbent cotton or glass wool loosened by water into a glass chromatograph tube (approx. 10 mm in inside diameter) by a thickness of approx. 5 mm, swell strong ba
34、sic anion exchange resin (Ci type 149 to 297 pm and 1.4 meq/ml min. in exchange capacity) with water, pour approx. 16 ml thereof in a slurry state and settle it. Thereafter, softly pack the absorbent cotton or glass wool loosened by water thereonto by a thickness of approx. 5 mm, pass 100 ml hydroch
35、loric acid (i + 5) and fill it into a resin column. Further, allow the flow rate of effluent to be not more than 5 ml per minute. An example of ion-exchange column is. shown in Attached Figure. Note ( 3 ) Because the outflow of effluent from an ion-exchange column differs according to the inside dia
36、meter of chromatograph tube, the particle size and capacity of ion-exchange resin, etc., the ion-exchange column shall be preliminarily regulated so that the outflow of effluent becomes not more than 5 ml per minute. Further, because a part of the conditions of adsorption, elution, etc, differs acco
37、rding to the type of ion-exchange resin, the flow rate of effluent, etc., it shall be preliminarily confirmed that iron, copper, etc. can be removed by washing in accordance with the operation of 5.2.5 (4). At the same time, the conditions of adsorption and elution of zinc are grasped by obtaining t
38、he curve of elution and zinc shall be confirmed to be able to be quantitatively eluted with a fixed amount of ammonia-ammonium chloride solution. 5.2.4 Weighing out Amount of Sample Weigh out a sample in accordance with Table 2 according to the content of zinc (+). Table 2 Weighing out amount Zinc c
39、ontent (%) 1 of sample (g) Note (4) Weigh out the sample so that the amount of zinc .does not exceed 150 mg. accordance with the following procedures: 5.2.5 Operation The determination operation shall be carried out in (1) Weigh out a sample, transfer it into a beaker (200 to 300 mi), cover it with
40、a watch glass, add 20 to 30 ml hydrochloric acid and vaporize sulfur in sulfides as hydrogen sulfide gas by gradually heating it. Thereafter, add 10 ml nitric acid (1 + 1) and decompose it by successively heating it (5)(6). Then, add 10 to 20 ml sulfuric acid (i + i), evaporate it by heating suffici
41、ently to gnerate white fume of sulfuric acid ( 7 ) and concentrate it to approx. 5 ml. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 20:28:35 MDTNo reproduction or networking permitted wi
42、thout license from IHS -,-,- J I S MrAl24 79 = 4933b08 00bb3b b 6 M 8124-1979 After standing to cool, add approx. 50 ml water and dissolve soluble salts by heating. After cooling it to room temperature, filter it by using a filter paper (Class 5 B) and wash it several times with sulfuric acid (1 + 1
43、00) (8). Receive the filtrate and washings with a beaker (200 to 3QO mi) and concentrate it by heating until the amount of solution becomes 60 to 80 ml. After standing to cool, add 16 ml hydrochloric acid, dilute the amount of solution to 100 ml with water and mix them by shaking. Pass this solution
44、 through an ion-exchange column at a flow rate of 5 ml per minute. After the solution disappears on the resin, use 100 ml hydrochloric acid (1 + 5 ) by dividing it in several times, wash the beaker, pass washings through the column at each washing and further successively pass 100 ml hydrochloric ac
45、id-ascorbic acid solution ( 9, and 100 ml hydrochloric acid (1 + 5). hitherto. Then, pass 180 ml ammonia-ammonium chloride solution at a flow rate of 5 ml max. per minute, elute zinc (10) and receive the effluent with a beaker (500 mi). Discard all the effluent Add 2 to 3 drops of p-nitrophenol solu
46、tion to this solution as indicator and neutralize it with acetic acid (i + i) until the color of solution turns from yellow to colorless. Then, add 20 ml acetic acid-ammonium acetate mixed solution, 3 ml ammonium fluoride solution and 5 ml sodium thiosulfate solution (11). Add 0.5 ml XO solution to
47、this solution as indicator, immediately titrate it with EDTA standard solution given in Table 3 and allow the point at which the color of solution turns from red purple to yellow to be the end point ( 12). Table 3 EDTA standard solution Zinc amount (mg) M/20 I 20 and over Under 30 I M/ 1 O0 Notes (
48、5 ) As to the sample for which the decomposition with nitric acid is suitable such as the sample containing a great amount of copper, lead, and iron sulfides or the like, after weighing out the sample, add 10 to 30 ml nitric acid and allow the sample to be decomposed by quietly heating it. ( 6 ) When the decomposition of deposited sulfur such as sulfides ore or the like, allow a small amount of bromine to be further added. (7) When a great amount of arsenic, antimony, tin or selenium is contained in a sample and affects on the determinating operation thereafter can not be neglected,