《JIS-K-0450-50-10-2004-ENG.pdf》由会员分享，可在线阅读，更多相关《JIS-K-0450-50-10-2004-ENG.pdf（20页珍藏版）》请在三一文库上搜索。
1、J IS JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association JIS K 0450-50-10 :zoo4 Testing method for benzophenone in industrial water and wastewater ICs 13.060.50 Reference number : JIS K 0450-50-10 : 2004 (E) PROTECTED BY COPYRIGHT 11 s Copyright Japanese Standard
2、s Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- K 0450-50-10 : 2004 Foreword This translation has been made based on the original Jap
3、anese Industrial Standard established by the Minister of Economy, Trade and Industry through deliberations at the Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law: Date of Establishment: 2004-01-20 Date of Public Notice in Official Gazette: 2004-01-20 Inv
4、estigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Environment and Recycling Policy JIS K 0450-50-10 : 2004, First English edition published in 2004-05 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JA
5、PAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 2004 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopyin
6、g and microfilm, without permission in writing from the publisher. Printed in Japan PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or net
7、working permitted without license from IHS -,-,- K 0450-50-10 : 2004 Contents Page 1 2 3 4 4.1 4.2 5 5.1 5.2 5.3 6 6.1 6.2 6.3 6.4 7 Scope Normative references Common matters . Sample . Sampling . Handling of sample . Pre-treatment of sample . Reagents Implement . Operation Gas chromatography mass s
8、pectrometry Reagents Apparatus Preparatory operation . Operation Marking of result . Attached Table 1 Normative references Annex 1 (normative) Column chromatograph separation by using activated magnesium silicate . Annex 2 (normative) Method of calculation for concentration by using sensitivity fact
9、or (RP) . Annex 3 (informative) Method of confirmation for the lowest limit value of determination range 1 1 1 3 3 3 3 3 4 6 9 9 9 10 10 12 13 14 15 16 PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing,
10、Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS K 0450-50-10 : 2004 Testing method for benzophenone in industrial water and wastewater 1 Scope This Japanese Industrial Standard specifies the testing
11、 method for diphenyl- methanone benzophenone (C13H100) (CAS No. 119-61-9)J in industrial water and wastewater from factory. 2 Normative references Standards listed in attached table 1 contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most recen
12、t editions of the standards (including amendments) shall be applied. 3 Common matters The common matters shall be as follows: General rule The general matters in common to chemical analysis shall be in accordance with JIS K 0050. Definitions For the purposes of this Standard, the definitions given i
13、n JIS K 0101, JIS K 0102, JIS K 0211 and JIS K 0215 apply. Gas chromatography mass spectrometry The general matter in common to gas chromatography mass spectrometry shall be in accordance with JIS K 0123. Designation of compound The designations of compounds, which are in ac- cordance with the namin
14、g scheme of compound established by the Chemical So- ciety of Japan the naming scheme of organic chemistry by International Union of Pure and Applied Chemistry (IUPAC), shall be used, and the idiomatic name shall be described with a parenthesis at the end, Determination range The determination range
15、 as shown in the testing method shall be expressed by the mass (pg) of target component in solvent introduced in a gas chromatograph mass spectrometer. Analytical precision The analytical precision shall be expressed by the coef- ficient of variation (Oro) which is obtained by the repeated tests at
16、the neighbourhood of the lowest limit of determination in the testing method(1). Note (1) Coefficient of variation (%) = -= X 100 S X where, s : standard deviation 2 : mean value Water The water to be used for a blank test, etc. shall be the water of A4 or A3 specified in JIS K 0557(2). Before using
17、, take 1 L of water into a separatory funnel, add 50 g of sodium chloride in 5 . 1 a) and 100 ml of hexane in 5 . 1 d), shake to mix them with using a vibrator for approximately 10 min, and leave it as it is. Carry out the opera- tion of 5 . 3 b) to d), j and k) however, the addition of naphthalene-
18、& internal standard solution (10 ygCloHs-ddml) in 5 . 1 i) is not carried out., take 1 pl of the concentrated solution with a microsyringe according to 6.4 a), introduce it into a gas chromatograph mass spectrometer, and confirm that the peak does not exist at the position corresponding to the reten
19、tion time of benzophenone (3). PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 K
20、0450-50-10 : 2004 Notes (2) For the water to be used for cleaning glassware, the water of A2 or A3 specified in JIS K 0557 may be used. (3) When refinement is required, it shall be in accordance with clause 4 Remarks 6 of JIS K 0557. Or, the water of A4 or A3 shall be treated with activated carbon,
21、etc. h) Reagents The common matters to reagents shall be as follows: i) The reagents, which are specified in JIS and do not hinder the test, shall be used. When not specified in JIS, the reagents without hindering the test shall be used. The concentration of the reference solution shall be expressed
22、 by mg/ml or pg/ml. The mixed solution of liquid reagents shall be expressed by reagent A- reagent B (a+b). This expression shall indicate that a ml of reagent A and b ml of reagent B are mixed. The concentration indicated with a parenthesis at the end of designation of the reference solution means
23、that it is the accurate concentration. The designations of reagents have been conformed to the naming scheme of compound established by the Chemical Society of Japan based on the naming scheme of inorganic chemistry and the naming scheme of organic chemistry by the International Union of Pure and Ap
24、plied Chemistry (IUPAC) and the designation of reagent in JIS as much as possible. For the compounds to be used for preparation of reference solution, the con- centration-known one shall be used. It is described as “reference mate- rial” in this Standard. The similar compounds are contained as impur
25、ities in them in many cases, therefore the one without hindering the test shall be used. The handling of reagents, wastewater, etc. shall follow the related laws and ordinance, etc., and care shall be sufficiently taken. 2) 3) 4) 5) 6) 7) i) Glassware The common matters to glassware shall be as foll
26、ows: 1) If not especially specified, the glassware specified in JIS R 3503 and JIS R 3505 shall be used. When a heating operation is accompanied, the boro- silicate glass-1 specified in JIS R 3503 shall be used. The desiccant to be used for a desiccator, if not especially specified, shall be silicag
27、el (4). The glassware to be used for the test, which are previously washed with water, shall be washed with acetone (not less than concentration 300 in quality specified in JIS K 8040), after volatilizing acetone by leaving as it is, heated at not less than 200 “C for not less than 2 h and left at t
28、he place being free from contamination as it is. Note (4) Type A class 1 of the silicagel desiccant for packing specified in JIS Z 0701 shall be used. 2) PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing
29、, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 K 0450-50-10 : 2004 j) Working curve The working curve shall be prepared within the determina- tion range so that the determination range as shown in the testing method is divided
30、 to 4 steps to 6 steps and the reference solution is taken so as to agree with the concentration at the time of introducing into the gas chromatograph mass spectrometer. 4 Sample 4.1 Sampling The sampling shall be as follows: 4.1.1 Implement The implement shall be as follows: a) Sample vessel, of 1
31、O00 ml of glass bottle with grounding stopper(5) Note (5j The bottle having a screwed stopper with tetrafluoroethylene resin pack- ing may be used instead of the grounding stopper. 4.1.2 Sampling operation The sampling operation shall be as follows: a) Sampling of surface layer water Take the sample
32、 according to 4.1.1 or 4.1.2 of JIS K 0094. b) Sampling of water at each depth Take the sample according to 4.1.4 of JIS K 0094. In addition to Bandone sampler, the one having the equivalent perfor- mance to this may be used. Sampling from a piping apparatus K 0094. cj Take the sample according to 4
33、.3 of JIS 4.2 Handling of sample Carry out the test immediately after sampled. If not carrying out immediately, preserve it in a dark place at O “C to 10 “C, and carry out the test as soon as possible. 5 Pre-treatment of sample After adding sodium chloride and benzophenone-dio to the sample and mixi
34、ng up to extract by adding hexane, concentrate the extracted solution. After letting the concentrated solution flow through the column chromato- graph tube used with silicagel and separating to let obstructive materials flow out, elute the target material with using acetone-hexane eluant, concentrat
35、e it again, add naphthalene-& and make a definite volume. When the obstructive material does not exist, the operation of column chromato- graph separation may be omitted. 5.1 Reagents The reagents shall be as follows: a) Sodium chloride, specified in JIS K 8150. After heating at approximately 600 “C
36、 for approximately 60 min, leave it cool in a desiccator as it is. Sodium sulfate, specified in JIS K 8987. After heating at approximately 600 “C for approximately 60 min, leave it cool in a desiccator as it is. Information : For sodium sulfate, PCB phthalic acid ester for test is on the market. b)
37、PROTECTED BY COPYEUGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 K 0450-50-10 : 2004 Acetone, of n
38、ot less than concentration 300 specified in JIS K 8040(6). Note (6) Before using, concentrate 200 ml to 1 ml according to the operation of 5.3 i) and k) however, the addition of naphthalene-& internal stan- dard solution (10 ygCloH8-ds/rnl) in i) is not carried out., take 1 p1 of the concentrated so
39、lution with a microsyringe according to 6.4 a), in- troduce it into a gas chromatograph mass spectrometer and confirm the absence of peak at the position corresponding to the retention time of benzophenone. Hexane, of not less than concentration 300 specified in JIS K 8825(6). Acetone-hexane eluant
40、(1+19), prepared by using acetone and hexane. Benzophenone-dl0 internal standard solution (100 pgC,sHloO-dldml-ac- etone) Take O. 100 g of benzophenone-dio (CisHoO-do) reference material into a 100 ml volumetric flask in which 2 ml to 3 ml of acetone has been previously contained, and add acetone up
41、 to the marked line. Take 10 ml of this solution into a 100 ml volumetric flask, and add acetone up to the marked line(7). Note (7) It shall be preserved at a dark place at below -5 O C . Benzophenone-dlo internal standard solution (10 gCi3HioO-didml-acetone) Take 1 ml of benzophenone-dlo internal s
42、tandard solution (100 pgCiJHioO-did mi) into a 10 ml volumetric flask, and add acetone up to the marked line(7). Naphthalene-& internal standard solution (100 pgCioH8-ddml) Take O. 100 g of naphthalene-& (ClOH8-dS) reference material into a 100 ml volumetric flask in which 2 ml to 3 ml of hexane has
43、 been previously contained, and add hexane up to the marked line. Take 10 ml of this solution into a 100 ml volumetric flask, and add hexane up to the marked line(7) (8). Note (8) This solution shall be used as the internal standard solution when the recovery of benzophenone-dl0 added to the sample
44、is obtained. Naphthalene-& internal standard solution (10 pgCioHs-dslml) Take 1 ml of naphthalene-ds internal standard solution (100 pgCoHs-ds/rnl) into a 10 ml volumetric flask, and add hexane up to the marked line(7) (8). Nitrogen, of grade 2 of high purity nitrogen specified in JIS K 1107. Implem
45、ent The implement shall be as follows: Separatory funnel, of 1 O00 ml to 2 O00 ml in capacity. Graduated test tube with grounding stopper, of 10 ml to 20 ml in capacity and graduated by 1 ml. Microsyringe, of 10 p1 to 200 p1, or automated introducing apparatus. Erlenmeyer flask with grounding stoppe
46、r, of 100 ml to 500 ml in capacity. Egg-plant type flask, of 100 ml to 500 ml in capacity with interchangeable ground joint and capable of connecting to a concentrator (rotary evaporator). Column chromatograph tube The column chromatograph tube shall be as follows. An example shall be as shown in fi
47、gure 1. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/16/2007 00:26:53 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 K 0450-50-10 : 2004 Tube
48、for column, of glass tube with cock having approximately 1 cm in inside diameter and approximately 30 cm in length. Column packing After heating the silicagel (9) for column chromatograph (particle diameter: 150 pm to 250 pm) at approximately 130 “C for approxi- mately 15 h, leave it cool in a desiccator as it is. Take 95 g of it into an Erlenmeyer flask with grounding stopper and drop 5 ml of water as stir- ring. Stopper it closely and mix gently until the finishing of heat genera- tion. Furthermore, shake to mix it by a vibrator for approximately 30 min. For the one p