1、BRITISH STANDARD BS 2690-117: 1983 Methods of testing Water used in industry Part 117: Long-chain fatty amines: spectrophotometric method IMPORTANT NOTE. It is essential that this Part be read in conjunction with the information in Part 100 of this standard, “Foreword, scope and general requirements
2、”, which is published separately. UDC 628.1:663.63.01:543.3:543.42.062:547.233BS2690-117:1983 This British Standard, having been prepared under the directionof the Environment andPollution Standards Committee, was published underthe authority of the BoardofBSI and comes intoeffecton 31 May 1983 BSI
3、07-1999 The following BSI references relate to the work on this standard: Committee reference EPC/37 Special announcement in BSINews March 1983 ISBN 0 580 11973 4 A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for
4、 their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages1 and 2, an inside back cover and a back cover. This standard has been updated
5、 (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date of issue CommentsBS 2690-117:1983 BSI 07-1999 i Contents Page 0 Introduction 1 1 Scope 1 2 Range 1 3 Principle 1
6、4 Interferences 1 5 Reagents 1 6 Treatment of apparatus 1 7 Sampling 1 8 Preparation of calibration graph 2 9 Procedure 2 10 Calculation 2 Publications referred to Inside back coverii blankBS2690-117:1983 BSI 07-1999 1 0 Introduction BS 2690-115, BS 2690-116 and BS 2690-117 together supersede BS 269
7、0-8:1969. This Part is a revision of clause 4. 1 Scope The method described is for the determination of long-chain fatty amines in industrial waters by a spectrophotometric method. 2 Range From 5 4g to 200 4g of long-chain fatty amine, expressed as octadecylamine, in a test portion not exceeding 100
8、 mL. 3 Principle The primary, secondary and tertiary forms of long-chain fatty amines react with methyl orange atpH 3 to 4 to form yellow complexes which are extracted into dichloromethane and determined colorimetrically. The calibration graph is prepared with the fatty amine that is added to the st
9、eam plant under investigation. As octadecylamine is the most commonly added fatty amine, it is used in the following method. 4 Interferences Cyclohexylamine, morpholine and ammonia do not interfere. Detergents interfere seriously and shall not be used for cleaning any glassware used in the test. 5 R
10、eagents 5.1 Buffer solution. Dissolve 125 g of potassium chloride and 70 g of sodium acetate trihydrate in500 mL of water. Add 300 mL of glacial acetic acid and dilute to 1 L with water. The pH value is 3.4. 5.2 Dichloromethane WARNING. Dichloromethane is harmful by inhalation. Avoid breathing its v
11、apour and contact with skin and eyes. 5.3 Propan-2-ol 5.4 Methyl orange solution. Dissolve 100 mg of methyl orange in 200 mL of water and add 50 mL of industrial methylated spirits (see 3.8 of BS 2690-100:1978). 5.5 Octadecylamine standard solutions 5.5.1 Octadecylamine stock solution. Weigh 0.500 g
12、 of octadecylamine into a 250 mL beaker, add 50 mL of glacial acetic acid and stir to dissolve. Transfer the solution to a 500 mL one-mark volumetric flask and dilute to the mark with water. Mix well. 5.5.2 Octadecylamine working solution. Dilute10.0mL of the octadecylamine stock solution(5.5.1) wit
13、h water to the mark in a1000mL one-mark volumetric flask(1mLN 104g of octadecylamine). Prepare this solution fresh before each calibration. 6 Treatment of apparatus Long-chain fatty amines tend to be absorbed on to glass surfaces and therefore all glassware apart from the optical cells shall be sili
14、cone-coated. This can be done by first cleaning the glassware with chromic acid and then rinsing the clean and dry surface of the glassware with a proprietary silicone emulsion, in accordance with the manufacturers instructions. The coating will usually last for about6 months and the glassware shall
15、 be re-treated when a normal water meniscus appears. 7 Sampling If the temperature of the water being sampled is above 30 C, the sampling line shall contain a small, permanently fixed, stainless steel cooling coil capable of reducing the temperature of the sample to about 25 C to 30 C. The sampling
16、line shall be kept as short as possible and the sample allowed to run to waste for at least 30 min before collection. Run the sample into a stoppered 250 mL silicone-coated glass bottle and analyse immediately.BS2690-117:1983 2 BSI 07-1999 8 Preparation of calibration graph Add 0, 1.0, 2.0, 5.0, 10.
17、0, 15.0 and 20.0 mL of the octadecylamine working solution (5.5.2) to a series of 150 mL separating funnels. This will correspond to 0, 10, 20, 50, 100, 150 and 200 4g of octadecylamine in a separating funnel. Treat the contents of each funnel as follows. Dilute to 100 mL with water, add 4.0 mL of t
18、he buffer solution (5.1), 2.0 mL of the methyl orange solution (5.4) and 20.0 mL of the dichloromethane(5.2), stopper and shake for 5 min. Invert the funnel and dry the stem with a spill of filter paper extending to the open tap. Close the stopcock and allow the funnel to stand upright for3min. Run
19、the dichloromethane layer into a dry50 mL separating funnel. Add 0.5 mL of the propan-2-ol (5.3) to the separated dichloromethane layer to remove any turbidity and swirl gently. Run off the dichloromethane into a 10 mm cell. Immediately measure the absorbance of the dichloromethane solution at a kno
20、wn temperature between 20 C and 25 C in a spectrophotometer at the wavelength corresponding to maximum absorption (approximately 430 nm, but the exact wavelength shall be checked for each spectrophotometer), using 10 mm cells. Use dichloromethane in the compensating cell. Deduct the reading for the
21、blank from those for the standard solutions and plot a calibration graph of absorbance against the number of micrograms of octadecylamine. The absorbance given by 200 4g of octadecylamine in the total volume of test solution is approximately1.2. 9 Procedure Measure a suitable volume of the sample (c
22、ontaining less than 200 4g of octadecylamine) into a 150 mL separating funnel and, if necessary, dilute to 100 mL with water. Add 100 mL of water to a second separating funnel to act as a blank. Treat the contents of each funnel as follows. To each funnel add 4.0 mL of the buffer solution(5.1), 2.0
23、mL of the methyl orange solution(5.4) and 20.0 mL of the dichloromethane(5.2), stopper and shake for 5 min. Invert the funnel and dry the stem with a spill of filter paper extending to the open tap. Close the tap and allow the funnel to stand upright for 3 min. Run the dichloromethane layer into a d
24、ry 50 mL separating funnel. Add 0.5 mL of the propan-2-ol (5.3) to the separated dichloromethane layer to remove any turbidity and swirl gently. Run off the dichloromethane into a 10 mm cell. Immediately measure the absorbance of the dichloromethane solution at the wavelength used for the calibratio
25、n graph and at a temperature within 1 C of that at which the calibration graph was prepared in the spectrophotometer. Use dichloromethane in the compensating cell. 10 Calculation Deduct the reading obtained for the blank from that for the sample and read off the octadecylamine content in micrograms
26、from the calibration graph. The concentration, in milligrams per litre, of octadecylamine is given by where m is the mass of octadecylamine from the calibration graph (in 4g); V is the volume of sample (in mL). m V -BS 2690-117:1983 BSI 07-1999 Publications referred to BS 2690, Methods of testing wa
27、ter used in industry. BS 2690-115, Cyclohexylamine: spectrophotometric method 1) . BS 2690-116, Morpholine: spectrophotometric method 1) . 1) Referred to in the introduction only.BS 2690-117: 1983 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national
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