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1、J I S R*22L2 9L m 4933bO 0507942 bTL m JIS JAPANESE INDUSTRIAL STANDARD Chemical analysis of refractory bricks and refractory mortars UDC 666.76:666.767:543 Translated and Published by Japanese Standards Association Printed in Japan 5 5 s Copyright Japanese Standards Association Provided by IHS unde
2、r license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S Rt22l12 71 m 4933b08 0507943 538 m In thc cvcnt or any doubt arising, the original Standard in Japanese is to be
3、final authority. a . . Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S R*K22L2 91 Y933608 0507944 47
4、4 D R 2212-1991 Contents Page 1 . Scope 1 2 . General matters 1 3 . Classes of chemical analysis of refractory bricks and refractory mortars 1 4 Sampling method 2 5 . Rounding off of analysis value and tolerance 2 . A . 1 . 2 . 3 . 4 . 5 . 6 . 7 . 8 . . 9 . 3 3 Chemical analysis of fireclay brick an
5、d fireclay mortar Method for determination of ignition loss Method for determination of silicon dioxide 3 Method for determination of aluminium oxide 8 Method for determination of ferric oxide 10 Method for determination of titanium dioxide 12 Method for determination of calcium oxide . 15 Method fo
6、r determination of magnesium oxide 20 Method for determination of sodium oxide . 21 Method for determination of potassium oxide 24 10 . Method for determination of manganese monoxide 26 B . 1 . 2 . 3 . 4 . 5 . 6 . 7 . 8 . 9 . Chemical analysis of silica brick and silica refractory mortar 28 Method f
7、or determination of ignition loss 28 Method for determination of silicon dioxide 28 Method for determination of aluminium oxide 34 Method for determination of ferric oxide 37 Method for determination of titanium dioxide 38 Method for determination of calcium oxide . 39 Method for determiantion of ma
8、gnesium oxide 42 Method for determination of sodium oxide . 44 Method for determination of potassium oxide 47 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or
9、networking permitted without license from IHS -,-,- R 2212-1991 Page 10 . Method for determination of manganese monoxide 48 C . Chemical analysis of high-alumina brick and high-alumina refractory mortar . 50 1 . Method for determination of ignition loss 50 2 . Method for determination of silicon dio
10、xide 51 3 . Method for determination of aluminium oxide 56 4 . Method for determination of ferric oxide 59 5 . Method for determination of titanium dioxide 60 6 . Method for determination of calcium oxide . 63 7 . Method for determination of magnesium oxide 69 8 . Method for determination of sodium
11、oxide . 71 9 . Method for determination of potassium oxide 74 10 . Method for determination of manganese monoxide 75 D . Chemical analysis of magnesite-brick and Magnesite refractory mortar 77 1 . Method for determination of ignition loss 77 2 . Method for determination of silicon dioxide 78 3 . Met
12、hod for determination of aluminium oxide 79 4 . Method for determination of ferric oxide 81 5 . Method for determination of calcium oxide 83 6 . Method for determination of magnesium oxide 86 . E . Chemical analysis of magnesite-chrome refractory brick and magnesite-chrome refractory mortar ( Contai
13、ning chrome refractory brick and chrome refractory mortar) 1 . Method for determination of ignition loss 2 . Method for determination of silicon dioxide 3 . Method for determination of aluminium oxide 4 . Method for determination of ferric oxide 5 . Method for determination of calcium oxide . 6 . Me
14、thod for determination of magnesium oxide 7 . Method for determination of chromium oxide . 87 87 88 91 94 97 100 101 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduct
15、ion or networking permitted without license from IHS -,-,- JIS R*22LZ 91 4933bO O507946 247 UDC 666.76:666.767:543 JAPANESE INDUSTRIAL STANDARD J I S Chemical analysis of refractory bricks R 2212-1991 and refractory mortars 1. Scope This Japanese Industrial Standard specifies the chemical analysis o
16、f refractory bricks and refractory mortars. Remarks: The following Standards are cited in this Standard: JIS K 0050-General Rules for Chemical Analysis JIS K 0115-General Rules for Molecular Absorptiometric Analysis JIS K 0121-General Rules for Atomic Absorption Spectro- chemical Analysis JIS K 8001
17、-General Rules of Testing Methods for Reagents JIS K 8005-Standard Substances for Volumetric Analysis JIS K 8885-Silicon Dioxide JIS Z 8401-Rules for Rounding off of Numerical Values JIS Z 8801-Test Sieves 2. General matters General matters common to the chemical analysis shall be in accordance As f
18、or reagents, guaranteed Classes of chemical analysis of refractory bricks and refractory mortars The chemical analysis of refractory bricks and refractory mortars shall with JIS K 0050, JIS K 0115 and JIS K 0121. grade reagents of JIS or those equal or superior thereto, shall be used. 3. be as follo
19、ws: (1) Chemical analysis of fireclay brick and fireclay mortar (2) Chemical analysis of silica brick and silica refractory mortar ( 3) Chemical analysis of high-alumina refractory brick and high-alumina refractory mortar (4) Chemical analysis of magnesite brick and magnesite refractory mortar (5) C
20、hemical analysis of magnesite-chrome brick and magnesite-chrome refractory mortar (containing chrome brick and chrome refractory mort ar) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:
21、41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S Rx2212 91 = 4933b08 0507947 i183 Item Ig. loss 0.05 Fireclay brick and fireclay mortar Silica brick and silica refractory mortar High-alumina refractory brick and high-alumina of over 98 % in 1203) High-alumina ref
22、ractory brick and high-alumina of under 50 % in A1203) Magnesite brick and mag- nesite refractory mortar 0.05 Ma nesite-chrome brick an8 magnesite-chrome re- taining chrome brick and chrome refractory mortar) 0.05 refractor mortar (those 0.05 refractor mortar (those 0.05 fractory mortar (con- 0.05 2
23、 R 2212-1991 SiO, A120, FeZ03 Tio, Ca0 MgO Na20 K 2 0 M n O Cr,O, 0.5 0.4 0.05 0.05 0.05 0.05 0.03 0.06 0.01 - 0.5 0.1 0.05 0.05 0.10 0.05 0.01 0.02 0.01 - 0.2 0.5 0.05 0.05 0.05 0.05 0.03 0.06 0.01 - 0.5 0.5 0.05 0.05 0.05 0.05 0.03 0.06 0.01 - - - - 0.15 0.5 - 0.20 0.05 0.05 - 0.30 - - 0.20 0.5 0.
24、30 - 0.15 0.5 - 4. Sampling method As for the analysis sample, grind all the test samples, pass them through 6.70 mm sieve of JIS Z 8801, take 100 g with a riffle sampler or by quartering and further grind all of them. totally passed through 300 um sieve by quartering. sample obtained by pulverizing
25、 more finely than the extent of totally passing through 90 um sieve in a flat weighing bottle (50 mm in diameter) and dry it in an air bath at 110 f 5OC for 2 h or more. a desiccator. 4.1 Take 10 g from the sample Thinly spread the Thereafter? reserve it in Take the sample therefrom. 4.2 In weighing
26、 out an analysis sample, weigh it out to the nearest 0.1 mg by using a chemical balance. 5. Roundine off of analvsis value and tolerance 5.1 As a rule, analyze the same sample twice. When the difference thereof is larger than the numerical value given in the tolerance (%) of Table 1, analyze the sam
27、ple again and allow average of numerical values obtained within the tolerance to be the analysis value. 5.2 In analysis, carry out a blank test over a l l the operation and correct the content rate. 5.3 Express the analysis results by percentage and round off in ac- cordance with JIS Z 8401 as follo
28、ws: (1) The first decimal place in the case where the content rate is an integer of two figures. (2) The second decimal place in the case where the content rate is an integer of one figure. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/11111110
29、01, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S R*= where, v,: used amount of M/100 EDTA standard solution in 6.2.4 (6) (mi) factor of M/100 EDTA standard solution f : W : weighing out amount of sample in 6.2.3
30、 (g) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S R*2212 91 m 4933b08 05079b2 I.19T m 17 R 2212-1
31、991 6.3 Atomic absorption method 6.3.1 Summary Decompose a sample with hydrofluoric acid and perchloric acid. After evaporating it to dryness, dissolve it with hydro- chloric acid and add lanthanum chloride to it to constant volume. Take a portion of this solution and measure the absorbance of calci
32、um by using absorption analyzer. Reagents The reagents shall be as follows: Hydrochloric acid (1 + 1) Nitric acid Perchloric acid (60 to 70 %) Hydrofluoric acid (46 %) Lanthanum chloride solution ( li) (1 + 1) to 50 g lanthanum oxide, dissolve it by heating and dilute it with water to 1 i . Add 200
33、ml hydrochloric acid Reserve it in a plastic bottle. Aluminium chloride solution (99.9 % min.), add 50 m l hydrochloric acid (1 + 1) and dissolve it by heating. After cooling, transfer it into a one mark volumetric flask of 500 ml and dilute it up to the marked line with water. aluminium oxide. Weig
34、h out 1.75 g metallic aluminium Allow 1 ml this solution to be equivalent to 6.6 mg Reserve it in a plastic bottle. Standard calcium oxide solution (0.5 mg CaO/ml) 0.892 g calcium carbonate and dissolve it with gradually adding 30 ml hydrochloric acid (1 + 1). After cooling, transfer it into a one m
35、ark volumetric flask of 1000 ml and dilute it up to the marked line with water. Weigh out Reserve it in a plastic bottle. Standard magnesium oxide solution (0.1 mg MgO/ml) 0.603 g metallic magnesium (99.9 % min.), gradually add 30 ml hydrochloric acid (1 + 1) and dissolve it by heating. cooling, tra
36、nsfer it into a one mark volumetric flask of 1000 ml and dilute it up to the marked line with water. it 10 times to be used. Weigh out After Accurately dilute Reserve it in a plastic bottle. Standard sodium oxide solution (0.5 mg Na20/ml) 0.943 g sodium chloride in water, transfer it into a one mark
37、 volumetric flask of 1000 ml and dilute it up to the marked line with water. Dissolve Reserve it in a plastic bottle. Standard potassium oxide solution (O. 5 mg K20/ml) 0.792 g potassium chloride in water, transfer it into a one mark volumetric flask of 1000 ml and dilute it up to the marked line wi
38、th water. Dissolve Reserve it in a plastic bottle. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S R
39、*22L2 91 M 4933608 0507763 32b M Aluminium Lanthanum Hydro- Calcium chloride chloride chloric soiution solution acid (1+1) oxide solution additional additional additional - amount amount amount Standard concen- ml mi m l :Enal tration amount mg/ m l 100ml 10 10 4 O O 10 10 4 1.0 0.5 18 R 2212-1991 M
40、agnesium Sodium oxide solution oxide SOlUtiOIl Standard concen- Fhdard concen- solution tration tration amount mg/ amount mg/ m l 100ml m l 100ml O O O O 1 . 0 o. 1 1 . 0 0 . 5 e e e e 10 10 (11) Standard mixed solution series-1 Stepwise take respective standard solutions of calcium oxide, magnesium
41、 oxide, sodium oxide, and potassium oxide into one mark volumetric flasks of 100 ml ( 12) , add 10 ml aluminium chloride solution, 10 m l lanthanum chloride solution, and 4 ml hydrochloric acid (1 + 1) to each of them and dilute them up to the marked line with water. Reserve them in a plastic bottle
42、s. Notes (11) Strontium chloride solution may be used. In that case, 122 g strontium chloride (6 hydrate) is dissolved in water, joined by 40 ml hydrochloric acid (1 + 1) and diluted to 1 I with water. It is reserved in a plastic bottle. The aliquot amount of each standard solution should preferably
43、 be of concentration equivalent to the content range of each component contained in the sample. Examples are given in Table 5. (I2) 10 4 8.0 4 . 0 8.0 0.8 8.0 4.0 10 4 9.0 4 . 5 9.0 0.9 9.0 4.5 Standard mixed solution Series-1 Potassium oxide solution Standard solution additional amount m l Concen-
44、tration mg/ 100 ml 1 O O 1 .o 0.5 2 2.0 1.0 3 4 3.0 1.5 4 . 0 2.0 5 6 2.5 5 . 0 6 . 0 7 3.0 7.0 3.5 a 9 8.0 4.0 9.0 4.5 10 6.3.3 Apparatus Use an atomic absorption analyzer. 6.3.4 Weighing out amount of sample Weigh out 0.2 g of sample. 6.3.5 Operation Carry out the determination operation in accord
45、ance with the following procedures: Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 01:41:31 MSTNo reproduction or networking permitted without license from IHS -,-,- JIS R*22L2 71 m 493360
46、8 0507764 262 m 19 R 2212-1991 Weigh out sample onto a platinum pan (for example, No. 751, moisten it with water, add 5 ml perchloric acid, 2 ml nitric acid, and 10 ml hydrofluoric acid, sufficiently mix them by stirring with platinum wire, carefully decompose it by heating on a sand bath, violently
47、 generate white fume of perchloric acid and evaporate it to dryness. After standing to cool, wash the inside wall of platinum pan with water, add 3 ml perchloric acid and violently generate white fume by heating again. When the sample becomes near dryness, thoroughly dry it up at a slightly lower te
48、mperature. Add 5 ml hydrochloric acid (1 + 1) and about 10 ml water, cover it with a watch glass and heat it on a water bath for about 10 min. After cooling, wash the watch glass with water to be removed, transfer it into a one mark volumetric flask of 100 ml (8), add 10 ml lanthanum chloride solution and dilute it up to the marked line with water. Allow this solution to be the sample solution (C) and utilize it for determination of calcium oxide, magnesium oxide, sodium oxide, and potassium ox