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1、i J I S M*8212 83 m 4933608 O066575 9 , UDC 622.341.1-14: 543.062: 546.72 JAPANESE I NDUSTRIAL STANDARD Methods for Determination of Total Iron in Iron Ores JE M 82 I 2-1983 Translated and Published Japanese. Standards Association Printed in Japan 10 s I Copyright Japanese Standards Association Prov
2、ided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*8212 83 W 4933608 0066576 O m Translation without guarantee standard in Japanese is to be evide
3、nce In the event of any doubt arising, the original Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- - !JIS
4、 M*8212 83 E 4933608 0066577 2 UDC 622.341. I- 14: 543,062: 546.72 JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of M 8212-1983 Total Iron in Iron Ores i. Scope This Japanese Industrial Standard specifies the method for determination of total iron in iron ores. 2. General Matters The
5、general matters common to the methods for determination shall conform to SIS M 8202. . 3. Division of Methods For determination of total iron in iron ores either of the following methods shall be used: (1) Method by stannous chloride reduction and potassium dichromate titration: Method by hydrogen s
6、ulphide reduction and potassium dichromate titration: Method by titanium trichloride reduction and potassium dichromate titration: This method applies to the whole range of total iron contents. (2) This method applies to the whole range of total iron. contents, (3) This method applies to the whole r
7、ange of total iron contents. Applicable Standards : JIS K 8005-Primary Standard Substances for Volumetric Determination JIS M 8202-General Rules for Chemical Analysis of iron Ores . Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User
8、=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- I J I S M*2L2 83 W 4933bO 0066578 4 2 M 8212-1983 4, Method by Stannous Chloride Reduction and Potassium Dichromate Titration 4 . 1 Summary Decompose a sample with suitable aci
9、d, and filter to make the filtrate main solution, Treat the insoluble residue with hydrofluoric acid, fuse with potassium disulphate, dissolve the melts in the hot water containing a small amount of hydrochloric acid, filter it by ammonia water precipitating iron hydroxide and the like, dissolving i
10、t in hydrochloric acid and combine the solution to the main solution. As for other method, fuse the sample with sodium carbonate and sodium peroxide, filter the melts precipitated in the hot water, dissolve the precipitate with hydrochloric acid. If necessary, oxidize the organic matter in the solut
11、ion with potassium permanganate. Then, reduce ferric iron to ferrous iron with stannous chloride and oxidize the excess of stannous chloride with mercuric chloride (11) . Adjust the acid concentration of this solution with mixed acid of sulphuric acid and phosphoric acid, and titrate with standard s
12、olution of potassium dichromate adding sodium diphenylaminesulphonate as the indicator. 4.2 Applicable Field In those cases where the sample is difficult to be decomposed with only hydrochloric acid, the sample is easy to be dissolved by roasting or the sample contains vanadium, the sample solution
13、shall be prepared by different methods. 4.3 Reagents Reagents shall be as follows: ( 1) Hydrochloric acid (2) Hydrochloric acid (2+1, 1+1, 1+2, 1+10, 2+100) (3) Hydrofluoric acid (4) Sulphuric acid (l+l) (5) (6) (7) Sodium hydroxide solution ( 2 /v %) (8) Ammonia water (9) Ammonia water (1+1) Mixed
14、acid (sulphuric acid 3, phosphoric acid 3, water 14) Boric acid solution (saturated, about 5 w/v %) ( 10) Potassium disulphate (potassium pyrosulphate) (11) Mixed fusing agents sodium carbonate (anhydride) 1, sodium peroxide 21 i . . : . - . _ . . . . . . . . . . . . . . o ,. . r -. , . . .- % . . I
15、. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- 1- J I S M*82L2 83 I 4933b08 00bb579 b E 3 M 8212-1983 (
16、12) Stannous chloride solution Place 200 ml of hydrochloric acid into a beaker (1000 mi), heat on a water bath, add 100 g of stannous chloride dihydrate (SnC12 2H20) little by little, after cooling, dilute with water up to 1000 ml. Place the solution into a brown bottle con- taining a small quantity
17、 of tin in granular or petal form to store, (13) Mercury (II) chloride solution (saturated, about 5 w/v %) ( 14) -Potassium permanganate solution (2.5 w /v %) (15) Ferric ammonium sulphate solution Weigh out 50 g of ammonium ferric sulphate (12 hydrate) (500 mi), dissolve it in sulphuric acid (1+19)
18、, and dilute with sulphuric acid (1+19) to 1000 ml. FeNH4( SOS), 12H201 , place into a beaker (16) N/10 standard solution of potassium dichromate (4.903 g K2Cr207/i ) Weigh accurately 4.903 g of potassium dichromate (K2Cr207)( JIS K 8005), place it into a beaker (300 mi), add about 100 ml of water t
19、o dissolve, place into a 1000 ml measuring flask, and dilute with water -up to the marked line. In this case , the solution shall not be standardized, and the purity indicated in the standard reagent shall be used as a factor to N / l O as it is. ( 17) Sodium diphenylaminesulphonate solution Dissolv
20、e O. 2 g of sodium diphenylaminesulphonate C6H5 NH C6H4 SOsNal in a small quantity of water and dilute with water to 100 ml. The solution shall be stored in a brown bottle. 4.4 Weight of Sample Taken 4.5 Procedure Sample for analysis shall be taken by 0.40 g. 4.51 Preparation of Sample Solution The
21、sample solution shall be prepared as follows : (1) When Sample Is Easily Decomposed with Hydrochloric Acid (1.1) Weigh a sample () (2) , place it into a beaker (300 mi), cover with a watch glass, add 40 ml of hydrochloric acid (2+1), place the beaker on low temperature zone (60 to 100OC) at a periph
22、ery of hot plate for about 1 h, transfer, then, the beaker to high temperature zone, and heat up to near boiling for about 10 min for decomposition Transfer the beaker from the hot plate, add warm water to make about 50 ml, filter the insoluble residue with a filter paper (Class 5 B), scrape and tra
23、nsfer the whole quantity of undissolved residue attached to the inside wall of the beaker on the filter paper by using a glass stick with rubber tube. Wash with warm hydrochlric acid (2+100) until yellow ColOur of ferric chloride on the paper disappears and wash, then, with warm water 6 to 8 times,
24、Collect the filtrate and washings in a beaker (500 mi), heat and concentrate it without boiling, then, reserve it as the main solution, I Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:
25、59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*8212 83 E 4933608 0066580 2 4 M 8212-1983 Place the insoluble residue with the filter paper into a platinum crucible (No. 30), dry, then incinerate by ignition, and allow to cool, Moisten the ignition residue wit
26、h sulphuric acid (l+l) , add about 5 ml of hydrofluoric acid, and heat gently to expel silicon dioxide and sulphuric acid. After cooling, add about 3 g of potassium disulphate, cover it, heat gently at first, and rise the temperature gradually to dark red to fuse the residue. After cooling, place th
27、e platinum crucible as it is into a beaker (300 mi), add about 100 m l of warm water and 5 ml of hydrochloric acid, heat gently to dissolve the melts, and take off the crucible after washing it with warm water. Add ammonia water little by little to alkalify slightly, heat to boil for a while, and tr
28、ansfer from the heater. Settle the precipitate Of ferric hydroxide and the like, filter with a filter paper (Class 5 A), and wash with warm water 6 to 8 times. Discard the filtrate and washings. Rinse with about 10 ml of hot hydrochloric acid (1+2) on the paper to dissolve the preci- pitate, and was
29、h firstly with warm hydrochloric acid (2+100) several times and then with warm water until the washings are free of acid. Collect the filtrate and washings to the original beaker, after dissolving the precipitates attached to the beaker and combine the solution with the main solution preserved in th
30、e procedure of 4.5.1 (1.1). (1.3) Add 5 ml of potassium permanganate solution (2.5 W / V %) and heat to a degree not to boil to oxidize organic matters. heating at near boiling point to evaporate it to about 30 ml. Notes (l) Continue In this method, coexistence up to 0.05 % of vanadium, 0.02 % of co
31、pper, and 2 % of chromium in a sample does not interfere. For a sample of remarkably hygroscopic property, it shall be in accordance with 3.2 (2) of JIS M 8202. (2) (2) When Sample Decomposition with Hydrochloric Acid Is Difficult but Sample Decomposition Is Possible by Addition of Stannous Chloride
32、 (2.1) Weigh a sample (l) (2), place it into a beaker (300 mi), cover with a watch glass, add 40 ml of hydrochloric acid (2+1), heat gently to decompose the sample as far as possible, add 10 ml of stannous chloride solution 4.3 (12) , successively heat at a low temperature, when yellow colour of fer
33、ric chloride appears in the solution, add a small excess of stannous chloride 4 . 3 ( 12) solution and continue heating. If necessary, repeat this pro- cedure until the sample is decomposed completely. Add, then, potassium permanganate solution (2.5 w /v %) drop by drop to oxidize excess of stannous
34、 chloride until yellow colour of ferric chloride appears in the solution, and heat near to boiling point for 10 to 15 min to expel chlorine. Transfer from the heater, allow to stand for cool, add warm water to make about 50 ml, filter the insoluble residue with a filter paper (Class 5 B ) , wash wit
35、h warm hydrochloric acid (2+100) until yellow colour of ferric chloride disappears from the paper, and wash with warm water 6 to 8 times. Collect the filtrate and washings in a beaker (500 mi), heat and concentrate, and then reserve it as the main solution. Copyright Japanese Standards Association P
36、rovided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproduction or networking permitted without license from IHS -,-,- I f 5 M 8212-1983 (2.2) Treat the insoluble residue according to the procedure 4.5.1 ( 1.2) and comb
37、ine with the main solution obtained in 4.5.1 (2.1). Treat it according to the procedure 4 . 5 . 1 ( 1 3). (2.3) (3) When Sample Decomposition with Hydrochloric Acid Is Difficult but Sample Decomposition Is Possible by Addition of Hydrofluoric Acid Weigh a sample (l), place it into a platinum dish (N
38、o. loo), add 20 ml of hydrochloric acid and 5 ml of hydrofluoric acid, heat gently without boiling while mixing with shaking the dish sometimes to dissolve, and concentrate until the surface of the solution is covered with a film. After cooling, add 10 ml of hydrochloric acid (1+1), heat to dissolve
39、 the salts, wash down the solution into a beaker (500 mi) with as small quantity as possible of water, heat until the yellow colourof ferric chloride appears, successively heat to evaporate and concentrate until the quantity of the fluid becomes about 30 ml. (4) When Sample Decomposition with Hydroc
40、hloric Acid Becomes Easy by Roasting (4.1) Weigh a sample () , place it into a porcelain crucible (Class 1 Type B , 30 mi) , roast and oxidize at 700 to 75OOC for 30 min, and allow to stand for cool. Transfer the contents into a beaker (300 mi) without brushing, wash the crucible with as small quant
41、ity as possible of water, further add 15 ml of hydrochloric acid, heat carefully not to boil, dissolve iron oxide sticked on the bottom of the crucible, place the solution to the beaker containing the sample. Wash the crucible with a small quantity of water and add 15 ml of hydrochloric acid in the
42、beaker. Cover with a watch glass, heat gently to decompose the sample, transfer from heater, add warm water to make the quantity of liquid about 50 ml, filter the insoluble residue with a filter paper (Class 5 B) , wash with warm hydrochloric acid (2+100) until yellow colour of ferric chloride disap
43、pears from the filter paper, then wash with warm water 6 to 8 times. Collect the filtrate and washings to a beaker (500 mi), heat to concentrate, and reserve this solution as the main solution. Treat the insoluble residue according to the procedure 4.5.1 (1.2) and combine with the main solution obta
44、ined in 4.5.1 (4.1). e (4.2) (4.3) Heat this solution at near boiling point to evaporate and to make about 30 ml. e Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:59:57 MDTNo reproducti
45、on or networking permitted without license from IHS -,-,- JIS M*8212 8 3 = 4933608 O066582 b CCI 6 M 8212-1983. (5) When Sample Contains Large Quantity of Vanadium ( 2, ( 3), place it into an alumina crucible () (Type C , 30 mi) , add Weigh a sample about 4 g of mixed fusing agent 4.3 ( li), mix wel
46、l, heat firstly at a low temperature. After melting, heat.at high temperature for fusion in dark red condition, and then allow to stand for cool, Place the crucible into a beaker (300 mi), add about 100 ml of warm water to dissolve the melts, heat to boil for several minutes, take off the crucible a
47、fter washing with warm water to preserve, cool the solution to the ordinary temperature in running water, filter the precipitates with a filter paper (Class 6), and wash with sodium hydroxide solution ( 2 W/v %) 6 to 8 times. Discard the filtrate and washings after this process. Rinse down the preci
48、pitates into a beaker (300 mi) by spray water, add 10 ml of hydrochloric acid, heat to dissolve, pour the solution on the original filter paper to dissolve the remaining preci- pitates, wash with warm hydrochloric acid (1+2) three times, then, with warm hydrochloric acid (2+100) several times, and finally, with warm water until the washings are free of acid, and then collect the filtrate and washings in a beaker (500 mi). Place the reserved crucible into the beaker to dissolve the remaining adhering substances, and take off the crucible after washing with