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1、J I S M*85L4 87 W 4733608 00bb7L b T- / UDC 622.363.4:669.162.1 J 543.062 JIS JAPANESE INDUSTRIAL STANDARD Methods for Chemical Analysis of Metallurgical Grade Fluorspar JIS M 8 5 1 4 - 1 9 8 9 Translated and Published by Japanese Standards Association Printed in Japan 18 S Copyright Japanese Standa
2、rds Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- I J I S M*85l14 89 4933b08 00bb972 8 In the event of any doubt arising, the origina
3、l 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, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS MS851
4、4 89 4933608 0066973 T I UDC 622.363.4:669.162.11543.062 JAPANESE INDUSTRIAL STANDARD J I S Methods for Chemical Analysis of M 8514-1989 Metallurgical Grade Fluorspar 1. Scope of calcium fluoride ( l), silicon dioxide ( l), calcium carbonate (l) , phosphorus , sulfur, arsenic, lead, and antimony in
5、metallurgical grade fluorspar. Note (l) The calcium fluoride, silicon dioxide and calcium carbonate, respectively fluorine, silicon, and carbon dioxide are determined to be converted to each type. This Japanese Industrial Standard specifies the methods for determination 2. Definitions The definition
6、s of principal terms used in this Standard shall be in accordance with JIS K 0050 and to others following definitions apply. (1) aliquot Accurate separation of solution by using a pipet. (2) to add V ml accurately Addition of v ml by using a buret. or a pipet. (3) to add ml Addition of Vml by using
7、a meter glass or the like. (4) to add about Vml By putting, on trial, solution measured pre- liminarily with a graduated cylinder into an appliance to be used, a same amount is judged by the eye and is joined. (5) to analyze independently Analysis by changing one or all of man and the date. 3. Gener
8、al Matters General matters common to the methods for chemical analysis shall be in accordance with the following Standards : JIS K 0050 JIS K 0115 JIS K 0121 JIS Z 8401 JIS Z 8402 4. Sampling and Treating of Analytical Sample 4.1 Original Sample for Analysis Prepare a sample by sampling by a method
9、specified between the delivery parties concerned, grind so that all thereof may pass through a standard sieve of 150 um (equivalent to 100 mesh), and take it as an original sample for analysis. Applicable Standards and Corresponding International Standards : See page 31. Copyright Japanese Standards
10、 Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- -_ - JIS Ma85IY 89 = 4933608 00bb74 I 2 NI 8514-1989 4.2 After sufficiently mixing an
11、original sample for analysis, spread widely, thinly about 40 g thereof on a porcelain flat-bottom evaporating dish or the like, dry in an air bath at 105 to llOC for 2 h, allow to stand to cool to room temperature in a desiccator, and take it as a sample for analysis. Sample for Analysis 4.3 Weighin
12、g of Sample For weighing out of an analytical sample, weigh out accurately an weighing out amount specified in each determination method from a sample for analysis to the nearest 0.1 mg by using a chemical balance. 5. Arrangement of Analytical Value independently. 5.1 Number of Analyses Analyze, as
13、a rule, a same sample two times 5.2 Indication of Analytical Value Indicate an analytical value by mass percentage to the mass of a weighed out sample, and round off to the lowest place of indication specified acocrding to an analytical component as follows in accordance with JIS Z 8401. (1) Compone
14、nts to be indicated to two places of decimals calcium fluoride , silicon dioxide and calcium carbonate. (2) Components to be indicated to three places of decimals phosphorus, sulfur, arsenic, lead, and antimony. 5.3 Investigation of Analytical Value Investigate the accuracy and precision of an analy
15、tical value as follows: (1) Investigation of Accuracy between the average value of an analytical result (2) of a standard sample obtained by analyzing independently in parallel two times a kind of the standard sample of which chemical characteristic is similar to an analytical sample and a standard
16、value, is less than a tolerance to the standard sample obtained from a standard deviation within the same laboratory indicated in each determination method by the formula (4.13) of 4.6.3 in JIS Z 8402, judge the accuracy of the analytical value obtained by simultaneous analysis to be satisfied. When
17、 the absolute value of the difference (2) Investigation of Analytical Precision in Same Laboratory When a range of two analytical results obtained by analyzing independently two times a same sample in a same laboratory is less than a tolerance within the same laboratory obtained from a standard devi
18、ation within the same laboratory indicated in each determination method in accordance with Table 1 of JIS Z 8402, judge the state to be no abnormal difference between those two analytical results. (3) Investigation of Analytical Precision between Different Laboratories In the case where results obti
19、aned by analyzing a same sample respectively independently two times in two different laboratories meet the condition of (2), when the absolute value of the difference between average values of respective two analytical results is less than a tolerance between different laboratories obtained from a
20、standard deviation indicated in each determination I Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- a a a
21、 a JIS M885L4 89 W 4933b08 OObb975 3 m 3 M 8514-1989 method in accordance with Table 1 of JIS Z 8402, judge the state to be no abnormal difference between analytical results in those two laboratories. Note (2) When any abnormal value exists, discard in accordance with Procedure 2 (1) of 4.5 in JIS Z
22、 8402. 5.4 Acceptance of Analytical Value Decide a final analytical value as follows : As a result from investigation for two analytical results obtained by analyzing independently two times an object sample and for two analytical results to a kind of standard sample executed parallel thereto, when
23、either of conditions of 5.3 (1) and 5.3 (2) are satisfied, judge the accuracy of analytical value and the analytical precision within the same laboratory to be no abnormality, and report the average value of two analytical results on the object sample to be a final value. In the case where a paralle
24、l analysis on a standard sample is impossible, when the results of investigation for two analytical results on an object sample meet the condition of 5.3 (2), report the average value of those two analytical results to be a final value. In the case where results of parallel analysis on a standard sa
25、mple do not meet the condition of 5 . 3 (i), regard the accuracy of all results of analysis performed simultaneously therewith as doubtful, discard all the analytical results on the object sample as a rule, and analyze two times again. In the case where two analytical results on an object sample do
26、not meet the condition of 5.3 (21, regard either one or all of those analytical results as doubtful, discard all those analytical results as a rule, and analyze two times again. In the case where two analytical results on an object sample do not meet the condition of 5.3 (2) and analysis is difficul
27、t to be performed again, treat according to 3.3.2 (1.2.2) of JIS Z 8402. 6. Method for Determination of Calcium Fluoride 6.1 Determination Method The method for determination of calcium fluoride shall be in accordance with evaporation thorium nitrate titrimetric method. This method applies to the sa
28、mple of all range in calcium fluoride content. 6.2 Evaporation Thorium Nitrate Titrimetric Method 6.2.1 Purport Add perchloric acid to a sample, perform steam distil- lation, and separate fluorine as hydrosilicofluoric acid. solution with a buffer solution, utilize Methylthymol Blue as an indicator,
29、 and titrate with thorium nitrate standard solution. Regulate pH of the Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license f
30、rom IHS -,-,- JIS M*:B514 89 = 4933b08 00bb97b 5 W 4 M 8514-1989 6.2.2 Reagents The reagents shall be as follows: (1) Perchloric acid (1.54 in specific gravity) (2) Buffer solution (3.5 in pH) Dissolve 94.5 g of monochloroacetic acid (CH2ClCOOH) and 207.4 g of sodium monochloroacetate (CH2ClCOONa) i
31、n water to 1 1 . (3) Standard fluorine solution (10 mgF/ml) sodium fluoride (NaF) dried at 5OOOC to constant weight, dissolve in water, transfer to a 1000 ml one mark volumetric flask by using water, dilute to the mark with water, and take it as standard fluorine solution. ethylene bottle to be rese
32、rved. Weigh out 22.104 g of Transfer this solution into a poly- (4) 0.025 mol/Z thorium nitrate standard solution Weigh out 13.803 g of thorium nitrate tetrahydrate Th (NO,), * 4H81 , dissolve in water, transfer to a 1000 ml one mark volumetric flask, and dilute to the mark with water. Standardize t
33、he factor of this solution as fol10 w s : Weigh out accurately 50 ml of the solution obtained by diluting standard fluorine solution accurately 10 times into a beaker (300 mi), and add water to about 200 ml. After adding 5 ml of buffer solution of (2) thereto, utilize Methylthymol Blue solution as t
34、he indicator, titrate with 0,025 mol/ 1 thorium nitrate standard solution, and calculate the factor (FI to O. 025 mol/ 1 from the following formula: where v;: used amount of standard fluorine solution diluted 10 times (mi) V, : used amount of 0.025 mol/ I thorium nitrate standard solution (mi) (5) M
35、ethylthymol Blue solution (io g/l) 6.2.3 Apparatus A fluorine distillation apparatus which is exemplified in Fig. 1 shall, as a rule, be used. (1) Steam Generater water and boiling tips. Still A flask of 250 ml to a main pipe of which a steam induction pipe and a thermometer are attached and to a by
36、 pass of which a dropping funnel is attached. A round-bottom flask (3000 to 5000 mi) containing (2) (3) Condenser A coiled condenser of 300 mm in length. (4) Heater a Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie N
37、ot for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS M*85L4 89 4933608 00bb977 7 5 M 8514-1989 Fig. 1. Fluorine Distillation Apparatus (An Example) Glass tube for Thermometer Steam generator, Heat er funnel receiver 6.2.4 Weighing out Amoun
38、t of Sample The weighing out amount of a sample shall be 0.20 g. 6.2.5 Operation The determination operation shall be carried out in accordance with the following procedures : (1) Distilling Separation Weigh out a sample, transfer to a still by washing with a small amount of water, and add several b
39、oiling tips. Thereafter, further add 35 ml of perchloric acid. After passing cooling water through a condenser, heat the still. When a temperature inside the still has reached 14OoC, introduce steam generated in a steam generator into the still ( 3). Continuously distill for 60 min at a speed of dis
40、tillate of about 4 ml per minute. After ending distillation, wash the inside of the condenser with a small amount of water, and joint to the distillate. Note ( 3 ) Preliminarily heat the steam generator to generate steam. However, do not introduce this steam into the still until a temperature inside
41、 the still reaches 140OC. (2) Titration Add 5 ml of buffer solution C6.2.2 (2)l to the solution obtained in (i), further add several drops of Methylthymol Blue solution as the indicator, titrate with O. 025 mol/ I thorium nitrate standard solution, and take the point at which the solution turns blue
42、 as the end point. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S M*85L4 89 m 4933608 0066978 9 m 6
43、 M 8514-1989 6.2.6 Measurement of Distilling Efficiency The measurement of distilling a efficiency shall, as a rule, be carried out according to the following procedures: Transfer accurately 5 ml of standard fluorine solution to a still. adding several boiling tips, further add 35 ml of perchloric a
44、cid. passing cooling water through a condenser, heat the still. in the stili has reached 14OoC, introduce steam generated in a steam generator into the still. distillate per minute for 60 min. After ending distillation, wash the inside of the condenser with a small amount of water, and joint to the
45、distillate. Hereinafter operate following the procedure of 6.2 5 (2). Calculate distillation efficiency (Rj from the following formula: After After When a temperature Continue to distill at a speed of about 4 ml in VXFXl.900 50 R= where v used amount of 0.025 mol/Z thorium nitrate standard solution
46、(mi) F : factor of 6.2.2 (4) 6.2.7 Blank Test Carry out the whole operation of 6.2.5 without using a sample, and obtain a blank test value. 6.2.8 Calculation Calculate calcium fluoride content in a sample from the following formula: o - VXFX0.003904X100 mXR Calcium fluoride wt/, - where v: used amou
47、nt of 0.025 mol/Z thorium nitrate after correction of blank test value (mi) F: factor of 6.2.2 (4) m.: weighing out amount of sample (g) I? : distillation efficiency 6.2.9 Analytical Precision The analytical precision by shall be as given in Table 1. his me Table 1. Analytical Precision ( 4 ) Unit:
48、wt% Standard deviation within Standard deviation between the same laboratory different laboratories O, 003 5 X CaF, (wt%) 3 +O. 190 3 -0.001 7 X CaF, (wt%) +O. 979 4 Note (4) The analytical precision herein is obtained by using the sample of 75.24 vit% or over to and excluding 98.17 Pt% in calcium fluoride content. hoc o e Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:33:39 MDTNo reproduction or networking permitted without license from IHS -,