《JIS-G-1327-1992-R2004-ENG.pdf》由会员分享，可在线阅读，更多相关《JIS-G-1327-1992-R2004-ENG.pdf（26页珍藏版）》请在三一文库上搜索。
1、JI$ UDC 669.15781 -198:543 JAPANESE INDUSTRIAL STANDARD Methods for chemical analysis of ferroboron Translated and Published by Japanese Standards Association Printed in Japan 14 S Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=
2、Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S GX1327 92 CQ q733hOB 053b72b bTB In the event of any doubt arising, the original Standard in Japanese is to be final authority. Copyright Japanese Standards Association Pr
3、ovided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- UDC 669.15781-198543 JAPANESE INDUSTRIAL STANDARD J I S Methods for chemical analysis of ferroboron G
4、 1327-1992 1. mination of boron, carbon, silicon and aluminium in ferroboron. Scope This Japanese Industrial Standard specifies the methods for the deter- Remarks: The following standards are cited in this Standard. JIS G 1301 General rules for chemical analysis of ferroalloys JIS K 8001 General rul
5、es of testing methods for reagents JIS Z 2615 General rules for determination of carbon in metallic ma te ri als JIS Z 8402 General rules for permissible tolerance of chemical analyses and physical test 0 2. mon with JIS G 1301. General requirements General requirement for this Standard shall be in
6、com- 3. Determination of boron 3.1 titrimetric method shall be specified in this standard for the determination of boron in ferroboron. This method covers the whole range of boron contents in ferroboron. Method for the determination of boron Ion exchange - sodium hydroxide 3.2 3.2.1 The sample is di
7、ssolved in mixed acid composed of nitric acid and hydrochloric acid. The undissolved residue is filtered and fused with mixed fusing agent composed of sodium peroxide and sodium carbonate, and dissolved in water. The solution is mixed in the filtrate. The coexisting ions such as iron, aluminium is s
8、eparated with an ion exchange resin. After mannitol is added, the solution is titrated with the standard sodium hydroxide solution. 3.2.2 (1) (2) (3) (4) (5) Mannitol Ion exchange - sodium hydroxide titrimetric method Summary of method Reagents The following reagents shall be used in this method. 0
9、Hydrochloric acid (1 + 1, 1 + 2, 1 + 100) Mixed acid (Hydrochloric acid 1 + nitric acid 3) prepared freshly just before use. Sodium hydroxide solution (40 gl, 4 gll) Mixed fusing agent sodium peroxide 7, sodium carbonate (unhydrate) 31 This solution shall be Its pH does not change when it is dissolv
10、ed in water(). Note (1 For removal of coexisting carbon dioxide gas, water which is heated to boil and cooled previously shall be used. (6) Ion exchange resin H type strong acid-cation exchange resin(2), the particle size shall be 250 pm or smaller(3). Copyright Japanese Standards Association Provid
11、ed by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS G*3327 92 m 4933608 0536728 470 m 2 G 1327-1992 Notes () Such a polystylene-sulforic acid type ion ex
12、changer resin shall be used as a strong acid-cation exchange resin. The methods of con- vertion to H type from Na type and regeneration of the used resin should be carried out as follows. Transfer about 200 ml of the swelled resin or the used resin to a beaker (500 mi). Add about 300 ml of hydrochlo
13、ric acid (1 + 2) and mix well for about 5 min. Separate the resin from hydrochloric acid (1 + 2), wash it with water and repeat washing until litmus paper does not turn to red. In the absence of any resin having desired particle size, arrange- ment of a size shall be carried out according to the fol
14、lowing method. Crush the resin, in small portions, in a porcelain mortor and screen it with sieves. Transfer about 150 ml of the sieved resin to a beaker (500 mi), add about 300 ml of water to swell the resin sufficiently and mix. Allow to stand a little while, separate to remove fine resin in the u
15、pper regions. Repeat above proce- dures several times with washing and obtain the resin of uniform particle size. (7) 0.1 mol/Z standard sodium hydroxide solution (4.000 g NaOHIZ) preparation and the storage of the solution, the method given in 4,4 (20.4) of JIS K 8001 shall be applied. For the The
16、standardization of this solution shall be as follows. Take 25 ml of standard boric solution (8) accurately in the beaker (500 mi) included 300 ml of water. Dilute the solution to about 200 ml with water. Adjust the pH of the solution to the value between 3.0 and 3.5 by sodium hydroxide solution (40
17、gil) with using a pH meter. Proceed as specified in (3.2) and (3.3) of 3.2.5 (3) and obtain the factor with the following equation. 25 F = - V where, F : the factor of 0.1 mol/Z standard sodium hydroxide V : the volume of 0.1 mol/Z standard sodium solution hydroxide solution (mi) (8) Standard boron
18、solution (0.001081 B g/ml) (H3B03) in about 500 ml of hot water, which was dried in a vacuum desiccator with magnesium perchloric to constant weight. Cool the solution to ordinary temperature, transfer it to a 1000 ml volumetric flask with water, and dilute to the marked line with water. Dissolve 0.
19、2 g of p-nitrophenol in 50 ml of methanol, Dissolve 6.184 g of boric acid (9) p-nitrophenol solution and dilute to 100 ml with water. 3.2.3 Apparatus and glassware used, as a rule. The following apparatus and glassware shall be Copyright Japanese Standards Association Provided by IHS under license w
20、ith JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 G 1327-1992 (i) Apparatus for dissolving the sample (refer to Fig. i) sisted of a round bottom flask (200 mi) with a ground glas
21、s joint and a reflux condenser. The condenser, in which water flows, is connected with the upper side of the round bottom flask. The column for ion exchange (refer to Fig. 2) The apparatus is consisted of a chromatograph column (with a glass filter), the lower end of which is fitted with a reservoir
22、 beaker (500 mi), and the upper end of which is fitted with a separating funnel (200 mi) for controlling the flow rate of the sample solution or the washings. acid-cation exchange resin 3.2.2 (611 swelled by water. Suck up the slurry with a polyethylene KOMAGOME pipett, of which the pointed end is m
23、ade thicker, and pour it from the upper end of the chromatograph column (a length of approx. 300 mm and an inside diameter of approx. 10 mm) with a slight gradient into the column until the length of the resin is piled up to approx. 150 mm, with settling down the resin by the appropriate volume of w
24、ater for preventing the formation of the air bubbles. The apparatus is con- (2j Add the appropriate volume of water to be a slurry in the H type strong a Fig. 1. An example of the apparatus for dissolving the sample Unit: mm Reflux condenser with a ground joint Round bottom flask with a ground joint
25、 (200 ml) a Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S G*3327 92 4933608 0536730 O29 4 G 1327-1
26、992 Pig. 2. An example of the ion exchange column Unit: mm 3.2.4 3.2.5 (i) (1.1) Weighing mass of the sample Procedure -_ - The mass of the sample shall he weighed 1.0 g. Procedu-re shall be carried out as allows. Preparation - of the sample solution Weigh the sample and transfer in a round bottom f
27、lask (200 mi) with ground glass joint. Connect the reflux condenser as shown in Fig. 1, add 20 ml of water into the round bottom flask from the upper inlet of the reflux condens- er and acid 18 ml of mixed acid 3.2.2 (a), in small portions. Boil to dissolve the sample gently for about 10 min after t
28、he initial violent reaction ceases, Cool, pour about 20 ml of water from the upper inlet of the reflux condenser and disconnect it from the flask after washing. Filter the sample solution contained in the round bottom flask into a beaker (300 mi) through the filter paper (class SB) and wash the prec
29、ipitate four to five times with hydrochlo- ric acid (1 -I- 100). Stock the filtrate anci the washing as a main solution. Transfer the precipitate with filter paper to a nickel crucible (30 mi) and heat gradually to burn off the paper. Allow to cool, loose the precipitate to the pieces thoroughly. Ad
30、d about 2 g of mixed fusing agent 3.2.2 (411 and mix well with the precipitate. First, heat the precipitate at a low tempera- ture and then fuse it thoroughly after gradually raising temperature to red (1.2) Chromatograph column with an ethylene tetrafluoride cock and a glass filter Inside diameter
31、: 0 10 Outside diameter : 12 H type strong acid- cation exchange resin / Glass filter (G-2) / Reservoir beaker (800 ml) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reprod
32、uction or networking permitted without license from IHS -,-,- JIS G*1327 92 q933bCl 0536733 Tb5 m 5 G 1327-1992 hot state. Allow to cool, add about 20 ml of warm water, by dividing into two portions, in the crucible and dissolve the melt. Filter the solution in a beaker (200 mi) through filter paper
33、 (class 6) and wash the crucible, the fil- ter paper and the residue with water sufficiently. Add 3 or 4 drops ofp-nitrophenol solution 3.2.2 (9)l as an indicator to the filtrate and the washing. Add hydrochloric acid (1 + 1) until the colour of the solution just changes from yellow to colourless. T
34、ransfer the solution and the main stocked solution to a 500 ml volumetric flask with water and dilute to the marked line with water. (1.3) (2) Separation with ion exchange resin prepared in (1) (1.3) in a beaker (300 mi). Pass the solution through the ion exchange column 132.3 (211 at the flow rate
35、of 5 ml per min. Wash the beaker (300 mi) taken out the sample solution with 200 ml of water several times and every time pass the washing through the ion exchange column. The effluent is received in a beaker (500 mi). Take 100 ml of the sample solution (3) Titration (3.1) (3.2) Adjust the pH of the
36、 solution prepared in (2) to the value between 3.0 and 3.5 with a pH meter by adding sodium hydroxide solution (40 gZ). Transfer the solution to the Erlenmeyer flask (500 mi) with a ground glass joint and connect the reflux condenser. Heat to boil the solution or about 2 min and cool. Transfer the s
37、olution to a beaker (500 mi) and adjust the pH to 6.9 by adding sodium hydroxide solution (4 gll) and hydrochloric acid (1 + 100) using a pH meter. Add 20 g of Mannitol 13.2.2 (511 to the solution and dissolve it with stirring well. Titrate the solution to pH 6.9 with 0.1 moVZ standard sodium hydrox
38、ide solution 13.2.2 (711. (3.3) 3.2.6 the reagents and the same procedure in accordance with 3.2.5 (1) to (3) in parallel with the determination of boron in the sample. Blank test Carry out a blank test using only the same quantities of all 3.2.7 tion. Calculation The boron content shall be calculat
39、ed with the following equa- (Vi - V2) x F x 0.001081 1 rn x - 5 Boron content wt% = where, Vi : volume of 0.1 mol/,! standard sodium hydroxide solution obtained in 3.2.5 (4) required for titra- tion of the sample solution (mi) V 2 : volume of 0.1 moVZ standard sodium hydroxide solution obtained in 3
40、.2.6 required for titration of the blank test solution (mi) solution F : factor of 0.1 mol/,! standard sodium hydroxide r n : weighing mass of sample (g) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale
41、, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S G*3327 92 w 4933608 0536732 9TL 6 G 1327-1992 3.2.8 Tolerance Trelance() shall be calculated as shown in Table 1. Table 1. Tolerance Unit: wt% Tolerance within a laboratory Tolerance between inter-l
42、aboratories 0.2 0.5 Note ( 4 ) Tolerances have been calculated from the results of cooperated experiments in accordance with JIS 2 8402. Tolerance within a laboratory is a tolerance calculated from the determination repeated twice in the same laboratory. Tolerance between inter- laboratories is the
43、corresponding arithmetic average calculated from the results of the determination repeated twice in the two spontaneous laboratories. 4. Determination of carbon 4.1 of the following methods. Classification of methods The determination of carbon shall be given by one (1) Titrimetric method after comb
44、ustion (2) Conductmetric method after combustion (3) Coulometric method after combustion This method shall be applicable to the This method shall be applicable to This method shall be applicable to the sample whose carbon content is not less than 0.05 wt%. the sample whose carbon content is not less
45、 than 0.001 wt%. sample whose carbon content is not less than 0.001 wt%. (4) Infrared absorptiometric method after combustion (integration method) This ifiethod shall be applicable to the sample whose carbon content is not less than 0.001 wt%. _ - - _ - I _ (5) Infrared absorptiometric method after
46、combustion (circulation method) This method shall be aiplicable to the sample whose carbon content is not less than 0.001 wt%. 4.2 Titrimetric method after combustion 4.2.1 Summary of method oxidizing carbon to carbon dioxide. After the carbon dioxide in the evolved gases is collected in standard so
47、dium hydroxide solution, the excess amount of the sodium hydroxide is titrated with standard suIfuric acid solution. The sample is burned in a stream of oxygen for 4.2.2 method. Reagent Reagents specified in 6.4.2 of JIS Z 2615 shall be used in this 4.2.3 5. of JIS 2 2615 shall be applied. The accel
48、erators shall be used the following Equipments and materials The equipments and the materials specified in materials. (1) Tin, pulverized such as 250 pm to 1000 pml. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 19:40:04 MDTNo reproduction or networking permitted without license from IHS -,-,- 7 G 1327-1992 Weighing mass of sample g Sample (2) Copper, pulverized such as 250 pm to 1000 pm. (3) Iron, pulverize