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1、 - J I S Kt0555 95 = 4933608 0529919 9TT . JIS UDC 628.1.038543.34i546.28-31 JAPANESE INDUSTRIAL STANDARD Testing methods for determination of silica in highly purified water JIS K Translated and Published by Japanese Standards Association Printed in Japan Copyright Japanese Standards Association Pr
2、ovided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:23:30 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*0555 95 m 4933608 0529920 bLL m In the event of any doubt arising, the original Standard in J
3、apanese 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, 03/14/2007 07:23:30 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS Kx0555 75 M 4733608
4、0529923 558 W UDC 628.1.038543.34546.28-31 JAPANESE INDUSTRIAL STANDARD J I S Testing methods for determination of silica K 0555-1995 in highly purified water 1. Scope determination of silica in highly purified water. This Japanese Industrial Standard specifies the testing methods for Remarks 1. The
5、se methods can be applied to the determination of silica contained in very pure water, too, other than highly purified water. 2, The standards cited in this Standard are listed in Attached Table 1. Matters in common The matters in common shall be as follows. General rules analysis shall follow JIS K
6、 0050. The general matters commonly applicable to chemical Absorptiometry shall follow JIS K 0115. The general matters commonly applicable to absorptiometry Electrothermal-type atomic absorptiometry applicable to electrothermal-type atomic absorptiometry (hereafter referred to as ?electrothermal ato
7、mic absorptiometry?) shall follow JIS K 0121. The general matters commonly Definitions follow those in JIS K 0101, JIS K 0102, JIS K 0211, and JIS K 0215. The definitions of main terms used in this Standard shall Range of determination shall be shown by the mass (pg) in the final solution, and that
8、by electrothermal atomic absorptiometry by the concentration (pg/Z) in the final solution. The range of determination by absorptiometry Precision of repeatability The precision of repeatability shall be shown by the variation coefficient (%) which has been obtained in repeated tests carried in the d
9、etermination range of each testing method (I). Note (l) Variation coefficient (%) = - X 100 o 5 where, o : standad deviation - x : average Water there is a specification in each procedure, follow it. Employ the water Al to A3 specified in JIS K 0557, but when Reagents Matters in common to reagents s
10、hall be as follows. (a) When reagent is specified in Japanese Industrial Standards, use the reagent which is the best one or is suitable one of the kind, and when there is no one specified in Japanese Industrial Standards, use the reagent giving no hindrance to test. Copyright Japanese Standards Ass
11、ociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:23:30 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K+0555 95 4933608 0529922 494 2 K 0555-1995 The concentration of solution of reagent
12、 is generally shown by g/Z (when reagent is compound, use the mass of anhydrous) or mol/Z. The concentration of reference solution, however, is shown by mg/ml or pg/ml. The concentration, given in parentheses behind the name of the solu- tion of reagent, means the approximate value except the case o
13、f reference solution. For instance, ascorbic acid solution (100 gil) means L(+)-ascorbic acid solution whose concentration is approxi- mately 100 g/Z. The concentration of liquid reagent is expressed by the mixing ratio with water reagent (a+b). This expression means mixing of a ml of reagent and b
14、ml of water, and can be used in case of nitric acid or sulfuric acid according to JIS K 0050. When these reagents are used not diluted, however, the name of reagent alone will do. When handling reagents, waste, or others, be sufficiently careful ac- cording to laws and regulations concerned. Glasswa
15、re and JIS R 3505. Glassware shall be principally the ones specified in JIS R 3503 The desiccant used in a dessicator shall be principally silica gel Note (2) Use silica gel desiccant for packing, type A class 1 specified in JIS Z 0701. Working curve (absorptiometry, electrothermal atomic absorptiom
16、etry) When a working curve is to be plotted, divide from 4 to 6 steps the determi- nation range shown in testing method, and take reference solution to suit these steps. Prepare the working curve to fall in the range of determination. In case of electrothermal atomic absorptiometry, use a newly plot
17、ted working curve when test is carried out, and when a lot of samples are tested successively) confirm indicated values, employing reference solution) timely in the middle of the test. In case of absorptiometry, the working curve, which has been plotted in advance, can be used. Environment for test
18、ment (for instance, in a clean room), which has cleanliness class 3 or higher specified in JIS B 9920. Carry out, preferably, these tests in the environ- Note, Remarks, and Figure numbered in each clause. Note, Remarks, and Figure shall be serially Marking of result test, testing method shall be att
19、ached. When there are 2 or more testing methods for making Remarks: At sampling and any procedure in testing, it is important to pay utmost attention not to get any contamination on the sample. Give consideration to the shape and material of used tools and their washing method. Be so careful that co
20、ntamination may not come from an ana- lyst. It is preferable to let him put on the gloves used in a clean room. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:23:30 MDTNo reproduction o
21、r networking permitted without license from IHS -,-,- JIS Kx0555 95 = 4933b08 0529923 320 D 3 K 0555-1995 Sampling Sampling shall be as follows. Container for sample tainer made of polyethylene, polypropylene, or polystyrene. The container for sample shall be the airtight con- Cleaning: of samde con
22、tainer (a) (b) Wash sufficiently sample container with Al water. Put Al water into a sample container by a quarter of its volume, stopper it, and shake violently for about 30 seconds to make washing. Repeat this procedure five times. Fill it with A3 water (or the same water as the water to be tested
23、), stopper closely it, allow it to stand for 16 hours or longer, and discard the water. Fill it with the same water as that at (c), stopper closely it, and allow it to stand until sampling is tried. (cl (d) Sampling procedures (a) Wash sufficiently with water the outlet of water purifying apparatus
24、or the end of sampling valve (1 of main piping, and fix a sample introducing pipe (made of soft synthetic resin) which has been suffi- ciently washed with A l water (2) previously. Discard the water in a sample container, and carry out the procedure in (2)(b) with the water to be tested. Make the en
25、d of a sample introducing pipe touch bottom of a sample container, let flow out sample by about 5 times volume of sample container, take out the sample introducing pipe, and stopper closely it after fully washing the stopper with sample. Notes (I) Sampling valve shall be made of anticorrosive materi
26、al such as stainless steel or the like. (2) When a sample introducing pipe has long distance, let flow out sample to completely displace the water staying from the sampling valve to the end of sample introducing pipe, and then further let flow out freely the sample for about 5 minutes successively.
27、In case of sampling from main pip- ing, it is preferable to let sample flow out always at the rate of about 1 Zlmin from the valve. (b) (c) Testing method For the determination of silica, either molybdenum-blue extraction absorptiometry or electrothermal atomic absorptiometry shall be adopted. 4.1 M
28、olybdenum-blue extraction absorptiometry Make ionic silica react with hexaammonium heptamolybdate to produce heteropoly compound, reduce it with L(+)-ascorbic acid to get molybdenum blue, extract it with 1-butanol, and measure the absorbance found in organic phase to determine silica. Determination
29、range: Precision of repeatability: Si02 0.5pg to 10 pg 5 % to 20 % by variation coefficient Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:23:30 MDTNo reproduction or networking permitt
30、ed without license from IHS -,-,- J I S K*0555 95 W V933b08 0529924 2b7 W 4 K 0555-1995 (i) Reagents bottles. Reagents shall be as follows, and they are stored in polyethylene Water A3 water or the water purified to the same level as this (it is preferable to distil water using a metal still). Use t
31、his water when preparing reagent solution for this test, and when carrying out opera- tions. Sulfuric acid (2.5 moll)-ammonium molybdate (188 g/Z) mixed solution Take about 300 ml of water, cool it, and add gradually 140 ml of sulfuric acid specified in JIS K 8951 while stirring it. Add the solution
32、, which has been prepared by dissolving 200 g of hexaammonium heptamolybdate tetrahydrate specified in JIS K 8905 in about 500 ml of water, into the above solution, after allowing it to cool at room temperature, transfer it into a 1000 ml measuring flask, and add water up to the marked line. Sulfuri
33、c acid (2+1) Take one volume of water in a beaker, cool it, and add gradually, while stirring it, 2 volumes of sulfuric acid speci- fied in JIS K 8951. Ascorbic acid solution (100 glZ) Dissolve 10 g of L(+)-ascorbic acid specified in JIS K 9502 in water to make total 100 ml. Store it in a dark place
34、 at 10C or lower, and never use it since it has colored. Sodium sulfate Specified in JIS K 8987. 1-butanol Specified in JIS K 8810. Silica reference solution (i mgSiOdml) (99.9 % or more) in an agate mortor, heat it at 700C to 800C for about 1 hour, and allow it to cool in a desiccator. Take its 0.5
35、00 g into a platinum crucible, add 4 g of sodium carbonate, reference mate- rial for volumetiric analysis, specified in JIS K 8005, mix them sufficiently, and heat to fuse it for about 40 minutes. After allowing it to cool, dissolve the melt in water, transfer it into a 500 ml mea- suring flask, and
36、 add water up to marked line. Grind sand-like quartz (l) Silica reference solution (50 pgSiOdml) ence solution (i mgSiO$ml) into a 500 ml measuring flask, and add Take 25 ml of silica refer- - water up to the marked line. Prepare this solution when it is needed. Silica reference solution (i pgSiO$ml
37、) Take 10 ml of silica refer- ence solution (50 pgSiOdm1) into a 500 ml measuring flask, and add water up to the marked line. Prepare this solution when it is needed. Note (l) Instead of quartz, granular silica (99.9% or more) may be used. In this case, carry out procedures as follows. Heat granular
38、 silica at 105C for about 1 hour, allow it to cool in a desiccator, take its 0.234 g into a platinum crucible, and thereafter similarly to the case of quartz, fuse it with add- ing 4 g of sodium carbonate, reference material for volumet- ric analysis, specified in JIS K 8005. (2) Implement and appar
39、atus Implement and apparatus shall be as follows. (a) Separatory funnel 300 ml, made of synthetic resin. (b) Photometer Spectrophotometer or photoelectric photometer Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie No
40、t for Resale, 03/14/2007 07:23:30 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S K*0555 95 M 4933608 0529925 I T 3 5 K 0555-1995 (3) Operation Operation shall be carried out as follows. (a) (b) Take 200 ml of sample (containing 0.5pg to 10 pg as Sioz) into a separato
41、ry funnel. Add 4 ml of sulfuric acid (2.5 mol/Z)-ammonium molybdate (188 g/Z) mixed solution, shake them, keep it at about 25“C, and allow it to stand for 20 minutes. Add 25 ml of sulfuric acid (2+1), shake them, add immediately 2 ml of ascorbic acid solution (100 g/Z), shake them (2), and allow it
42、to stand for 10 minutes. Add 25 ml of 1-butanol, and extract molybdenum blue by means of shaking it for about 2 minutes. After standing, put 1-butanol layer into a test tube with a ground stopper, and add sodium sulfate to make dehydration. Transfer it into a 20 mm absorption cell (9, and measure it
43、s absor- bance in the vicinity of 800 nm wavelength with making 1-butanol contrast solution. Carry out the following procedures to obtain a blank test value based on the sulfuric acid (2.5 mol/Z)-ammonium molybdate (188 g/Z) mixed solution which will be added by the procedure below, and correct the
44、absorbance obtained on treating sample. Put respectively 200 ml of water into (A) and (B) of separatory funnel, and put 4 ml of sulfuric acid (2.5 mol/Z)-ammonium molyb- date (188 glZ) mixed solution into (A) and 8 ml of the solution into (BI, and shake them. Keep the solution at about 25“C, and all
45、ow it to stand for 20 minutes. Then, carry out the procedures from (c) to (f), and measure the absorbances of (A) and (B), to make respectively the value “u“ and “b“. According to the following formula, the blank test value IC“ on the basis of sulfuric acid (2.5 mol/Z)-ammonium molybdate (188 gll) m
46、ixed solution shall be calculated. (c) (d) (e) (0 (g c = b - a (h) Find the amount of silica on the working curve, and calculate the concentration of silica (pgSiOzlZ) in sample. Working curve ence solution (i pgSiOdm1) into as many separatory funnels, add water (4 to make total 200 ml, and carry ou
47、t the procedures from (b) to (f). Separately, take 200 ml of the same water as that used in this procedure, carry out the procedures from (b) to (f), and correct the absorbance obtained on the silica reference solution, and plot the relation curve between amount of silica (Sioz) and absorbance. Note
48、s (2) After adding sulfuric acid (2+1) and shaking them, immedi- ately add ascorbic acid solution (100 gil) and shake them. (3) If the concentration of silica in sample gives 10 pgSi0dZ or over, employ a 10 mm absorption cell. However, also in case of a blank test or plotting working curve, a 10 mm
49、absorbtion cell shall be used to measure absorbance. When plotting a working curve, take stepwise from 1 ml to 10 ml Take stepwise from 0.5 ml to 10 ml of silica refer- Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/20