1、BRITISH STANDARD BS 5117-1.3: 1985 Testing corrosion inhibiting, engine coolant concentrate (“antifreeze”) Part 1: Methods of test for determination of physical and chemical properties Section 1.3 Determination of freezing point NOTEIt is recommended that this Section be read in conjunction with the
2、 information given in the “General introduction”, published separately as BS 5117-0. UDC 661.17:621.43 715.4:620.197.3BS5117-1.3:1985 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comes in
3、toeffect on 28 June 1985 BSI 07-1999 First published, as BS 5117, December 1974 First part revision, Section 1.3, June 1985 The Committees responsible for this British Standard are shown inPart 0 The following BSI references relate to the work on this standard: Committee reference CIC/7 Draft for co
4、mment 83/55151 DC ISBN 0 580 14354 6 A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summ
5、ary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages1 to4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside fron
6、t cover. Amendments issued since publication Amd. No. Date of issue CommentsBS5117-1.3:1985 BSI 07-1999 i Contents Page 1 Scope 1 2 Principle 1 3 Reagents 1 4 Apparatus 1 5 Sampling of the product and preparation of test solution 2 6 Procedure 2 7 Preparation of cooling graph 2 8 Expression of resul
7、ts 2 Figure 1 Apparatus for determination of freezing point 1 Figure 2 Typical cooling graphs 3 Publications referred to Inside back coverii blankBS5117-1.3:1985 BSI 07-1999 1 1 Scope This Section of BS 5117 describes a method for the determination of the freezing point of solutions of engine coolan
8、t concentrate. NOTE 1The engine coolant concentrate is referred to hereafter as “the product”. NOTE 2The method as described is intended for the determination of the freezing point of solutions prepared from the product as supplied but the procedure may be adapted for solutions obtained from engine
9、cooling systems, test rigs, etc. NOTE 3The titles of the publications referred to in this standard are listed on the inside back cover. 2 Principle A test portion is cooled under specified conditions; a cooling graph is plotted from which is obtained the freezing point. 3 Reagents 3.1 General. The r
10、eagents used shall be of a recognized analytical grade. Water complying with BS 3978 shall be used throughout. 3.2 Propan-2-ol 3.3 Solid carbon dioxide 4 Apparatus 4.1 General. The apparatus described in 4.2 to 4.8 is required. The items described in 4.4 to 4.7 are shown in Figure 1. 4.2 One-mark vo
11、lumetric flask, of 100 mL capacity, complying with class A of BS 1792. 4.3 Burette, of 50 mL capacity, complying with classA of BS 846. 4.4 Cooling bath, consisting of a Dewar flask, capacity approximately 2 L, firmly mounted in a close fitting container and containing a pad of glass wool. 4.5 Test
12、portion holder, consisting of an unevacuated, unsilvered Dewar flask, capacity200mL, fitted with a stopper through which are bored three holes. The central hole accommodates the thermometer (4.6), and the side holes permit the passage of the stirrer (4.7) and the seeding wire (4.8). The latter hole,
13、 6 mm to 7 mm in diameter, is closed with a stopper when not in use. 4.6 Thermometer, designated A10C/100, complying with BS 593, mounted so that the tip of the bulb is about 10 mm from the base of the test portion holder (4.5). 4.7 Vertically agitated stirrer, mechanically operated, made of stainle
14、ss steel wire1.6mmdiameter, having five coils spaced so as to remain totally immersed in the test portion during the determination. Its action is such that it just clears the base of the test portion holder (4.5) at the bottom of its vertical stroke. 4.8 Seeding wire, made of stainless steel, by mea
15、ns of which small quantities of frozen test solution may be introduced into the test portion during the determination. Figure 1 Apparatus for determination of freezing pointBS5117-1.3:1985 2 BSI 07-1999 5 Sampling of the product and preparation of test solution 5.1 Sampling Take a representative sam
16、ple of not less than500mL, preferably from previously unopened containers in which the product is normally offered for sale 1) . Place the sample in clean, dry, stoppered glass bottles of a dark colour. Agitate all containers before sampling to ensure homogeneity of the contents. Where a batch of co
17、ntainers is to be sampled, it is essential that the number of containers sampled is not less than the cube root of the number of containers in the batch. Prepare the final sample by taking equal portions from each container sampled and mix them together thoroughly. Take care to ensure that any metho
18、d used for sealing the sample does not cause contamination. NOTEA series of different tests may be carried out by using separate portions taken from one sample. 5.2 Preparation of test solution Prepare the test solution at 50 % (V/V) concentration, or as otherwise specified, as follows. Using the bu
19、rette (4.3) measure accurately the required volume of the sample into the one-mark volumetric flask (4.2) and make up to the mark with water. Stopper the flask and invert it several times to mix the solution. 6 Procedure Assemble the apparatus. Fill the cooling bath (4.4) surrounding the test portio
20、n holder (4.5) with some of the propan-2-ol (3.2) and add small lumps of the solid carbon dioxide (3.3) to lower the temperature of the cooling bath to about 8 4 C to 10 C below the anticipated freezing point of the test solution (5.2). Ensure that a layer of the solid carbon dioxide at least 13 mm
21、thick is maintained in the cooling bath throughout the determination. Temporarily remove the stopper from the test portion holder (4.5) and add a test portion of about80 mL of the test solution (5.2), the approximate freezing point of which has previously been determined by cooling rapidly. NOTEThe
22、test portion may be precooled to about 8 C above the anticipated freezing point immediately prior to the determination. Start the stirrer and adjust its rate of stirring to about 60 to 80 strokes/min. Observe the temperature of the test portion at this point and thereafter record the temperature at
23、30 s intervals, increasing the frequency of recording (if possible to once every 15 s) towards the anticipated freezing point. At the anticipated freezing point, seed the test portion (to prevent supercooling) by introducing a small quantity of the test solution (5.2), frozen on to the tip of the se
24、eding wire (4.8). At this stage the rate of cooling shall be less than 1 C/min. Continue recording the temperature for at least10min after the apparent freezing point. 7 Preparation of cooling graph Plot a graph having, for example, the temperature, expressed in C, as ordinates and the time, express
25、ed in minutes, as abscissae. Typical graphs are shown in Figure 2, the effect of supercooling being illustrated in Figure 2(b). 8 Expression of results The freezing point, expressed in C to one place of decimals, is read from the cooling graph as shown in Figure 2. 1) See A.2 of BS 5117-0:1985 and c
26、lauses 4 and 5 of BS 3195-1:1978, for further guidance on sampling procedures and equipment.BS5117-1.3:1985 BSI 07-1999 3 Figure 2 Typical cooling graphs4 blankBS5117-1.3:1985 BSI 07-1999 Publications referred to BS 593, Laboratory thermometers. BS 846, Specification for burettes. BS 1792, Specifica
27、tion for one-mark volumetric flasks. BS 3978, Water for laboratory use. BS 3195, Methods for sampling petroleum products. BS 3195-1, Liquid hydrocarbons: manual sampling. BS 5117, Testing corrosion inhibiting, engine coolant concentrate (“antifreeze”). BS 5117-0, General introduction. BS 5117-1.3: 1
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