1、- STDmBSI BS EN IS0 9665-ENGL 2000 bb24bb9 138813039 493 BRITISH STANDARD Adhesives - Animal glues - Methods of sampling and testing (IS0 9665:1998) The European Sandard EN IS0 9665:ZOOO has the status of a British Standard 5s EN IS0 1665:2000 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITIED BY
2、 COPYBIGiT LAW STD.BSI BS EN IS0 SbbS-ENGL 2000 Lb24bbS 0880040 105 BS EN IS0 96652000 been prepared under the Committee for Materiais and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 October 2 direction of the Sector Amd.No. Date O BSI 10-2000
3、ISBN O 580 36591 3 National foreword Comments This British Standard is the official English ia,nguage version of EN IS0 9665:2000. It is identical with IS0 9665:1998. It supersedes BS EN IS0 9665: 1995 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee P
4、Ry52, Adhesives, which has the responsibility to: - aid enquirers to understand the text; - present to the responsible intedonaVEuropean committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; - monitor related intedonal and European developments a
5、nd promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications wit
6、h their corresponding European publications. The British Standards which implement intedonal or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “Intem from containers of less than 50 kg of glue take a proportionate amount. Thi
7、s sample is called the preliminary sample. Take appropriately sized samples by means of a sampling tube, scoop or similar tool to ensure that glue is taken from the top, middle and bottom of the container. Store these preliminary samples in clean, dry, airtight, non-absorbent containers until requir
8、ed. NOTE - For further guidance, reference should be made to IS0 3951:1989, Sampling procedures and cham for inspection by variables, for percent nonconforming, and IS0 821 3: 1986, Chemical products for industrial use - Sampling techniques - Solid chemical products in the form of particles varying
9、from powders to coarse lumps. 4.3 Final selection of sample Mix the preliminary samples thoroughly and take one or more samples from the bulk, each weighing not less than 1 kg, and store them in clean, dry, airtight, non-absorbent containers. These samples shall be known as the laboratory samples. 5
10、 Preparation of test sample 5.1 Reduction of solid (powdered, pearl, cube and granulated) glue sample Grind the sample by hand in a mortar, or alternatively in a laboratory disintegrator, of a type capable of grinding the sample to a particle size of 3 mm or smaller. This sample is called the test s
11、ample. If necessary, quarter this sample in the usual manner to bring the final mass to 500 g, taking care that a representative amount of all particle sizes is included in the quartering. Keep the powdered samples so obtained in two air-tight containers, one container for the test sample for moistu
12、re content (see clause 6) and the second container for all other tests. The type of disintegrator used to grind the sample shall be agreed on between the purchaser and vendor because different types of disintegrator generate different amounts of heat and have different effects on the moisture conten
13、t of the sample. Because of the loss of moisture in grinding, take a separate sample for the moisture content test from the material obtained by the preliminary breaking up, before the material is put through the disintegrator. This small separate sample is then powdered by hand in a mortar and pest
14、le, or cut with scissors, and is suitable for the moisture content test. Make adjustment for the moisture content of the mechanically ground sample by comparison with the hand-ground sample, which is considered as having the more reliable moisture content. By comparing the actual moisture content fo
15、und on the hand-ground sample with the moisture content of the mechanically ground sample, the necessary adjustment to be made to the mass of the glue to be used in the various tests is determined by calculation. 2 Place all samples immediately into an air-tight container because even a small change
16、 in the moisture content will affect the result of some of the tests; for example, an increase of 1 % moisture will result in a decrease of about 2,5 % in gel strength when determined on the Bloom-type gelometer. 5.2 Concentrations for solid glues Table 1 summarizes the mass of glue and volume of wa
17、ter required for each of the tests described. Weigh the specified quantity of the powdered sample for each test separately, rather than by working from a large quantity of stock solution. Table 1 - Glue concentrations Clause 6 7 8 9 10 11 12 13 14 16 lest Moisture content Gel strength (see 7.5.2) Co
18、mparison of gel strength viscosity Softening point Setting point Foam PH Grease Keeping quality Mass of glue 9 1 15 (7,5) 5to10 15 37,5 37,5 5 1 10 20 Volume of water ml 10 105 (105) 50 105 75 75 50 1 O0 15 80 5.3 Dissolving solid glues Weigh the test portion in a beaker and add the requisite amount
19、 of cold distilled water, stirring with a thin metal or glass rod. Place a watch glass over the mouth of the beaker and allow the sample to soak for 2 h at a temperature not exceeding 22 OC. Heat the beaker in a water bath adjusted to a maximum temperature of 70 “C for about 15 min, taking care that
20、 the final temperature of the solution when in the bath reaches, but does not exceed, 60 “C. During this heating period, gently stir the solution with the rod. Take care that the glue is completely dissolved: this may be ascertained by lifting up the beaker and inspecting its contents through the bo
21、ttom. When the test portion has all dissolved, remove the beaker from the water bath. If the sample gives a gel strength above 400 g Bloom, prepare the gel at a concentration of 6,67 %, and note this observation in the report. The results on a 6,67 % solution are sometimes expressed as “single Bloom
22、“, and those on a 12.5 YO solution as “double Bloom“. 6 Determination of moisture content 6.1 Principle A weighed test portion of the glue is maintained at 105 “C for 18 h and is then reweighed. 6.2 Apparatus 6.2.1 Stainless-steel dish, flat-bottomed, 70 mm in diameter and 15 mm high, weighing about
23、 30 g, preferably fitted with an aluminium cover for use when cooling and weighing. 3 6.2.2 Oven, capable of being maintained at 105 OC f 1 OC. 6.2.3 Water bath. 6.2.4 Balance, capable of weighing to the nearest 0,Ol g. 6.2.5 Desiccator 6.3 Procedure Weigh into the tared dish (6.2.1), to the nearest
24、 0,Ol g, about 1 g of the test sample for moisture content (see 5.1, third parag rap h). Add 10 mi of distilled water and allow the glue to soak. Place the dish on a warm water bath (6.2.3) so that the glue is dissolved and a homogeneous solution obtained and leave there until most of the water has
25、evaporated, giving a uniformly thin film. Transfer the dish to the oven (6.2.2) set at 105 OC tr 1 OC, and allow it to remain there for 18 h f 1 h, during which time the oven door shall not be opened. Remove the dish from the oven and, after allowing it to coo1 in a desiccator (6.2.5), weigh it. Car
26、ry out the determination in duplicate. 6.4 Expression of results Calculate the moisture content (M) as a percentage by mass, using the equation: M= mo -ml x100 m0 where mo is the initial mass, in grams, of the test portion; ml is the mass, in grams, of the test portion after drying. Express the resu
27、lt as the mean of the two values obtained in the duplicate determination. 6.5 Test report The test report shall include the following information: a) a reference to this International Standard; b) all details necessary for the complete identification of the glue tested; c) the number of containers s
28、ampled and the mass of glue taken from each container; d) the results of the test, including the individual values, and any circumstances that may have affected the results. 4 STDoBSI BS EN IS0 Sbb5-ENGL 2000 M Lb24bbS 0880050 054 = EN IS0 9665:2000 6.6 Variation of gel strength and of viscosity wit
29、h moisture content If greater precision is required, adjust the result to allow for variations in the moisture content. An approximate formula for the change in gel strength (AF) as a result of a change in moisture content (AM) is: -2fixAM AF= 100 - Ml where F1 is the gel strength at a percentage mo
30、isture content MI. This formula may be used to calculate the gel strength of glue at an agreed moisture content, e.g. 15 %. NOTE - If Ml is taken as 15 Yo, then AF = F/42,5 for each 1 % change in moisture content. As an example of the scale of this effect, an increase in moisture content from 15 % t
31、o 16 % reduces the measured gel strength of a 250 g gel strength glue by 6 g- There is no satisfactory formula for the change of viscosity, Av, with moisture content, AM, but a rough guide is given by AM Av = - 2,6171 x - 1 O0 This formula applies to 123 % solutions of glue. 7 Measurement of gel str
32、ength 7.1 Principle The gel strength of the sample for the test is measured under arbitrary conditions. A suitable instrument measures the force necessary to give a 4 mm depression in a gel of 123 % concentration by mass, matured for 16 h to 18 h at 1 O OC, using a standard plunger (7.2.4). By conve
33、ntion, this force has normally been expressed as a mass in grams (see, however, 7.6). 7.2 Apparatus 7.2.1 Wide-neck bottle, of internal diameter 59 mm k 1 mm, approximately 85 mm high, having a capacity of approximately 155 ml. The bottle shall have a stopper approximately 43 mm in diameter, pierced
34、 centrally with an air vent about 2,5 mm in diameter. 7.2.2 Thermostatically controlled bath, capable of being maintained at 65 OC f 1 OC. 7.2.3 Totally enclosed thermostatically controlled bath, fitted with a thermometer, and capable of being maintained at 10 OC f 0,l OC. 7.2.4 Plunger, made of a s
35、uitable, stable polymer with a diameter of 12,7 mm and an edge radius of 0,39 mm k 0,04 mm (see figure 1). NOTES I 1 The diameter of the plunger and its edge radius are mandatory; other dimensions are for guidance only. 2 Some types of commercially available apparatus may have plungers that do not c
36、onform to the dimensions specified for the diameter and edge radius, and it is essential that compliance, particularly with reference to the radius of curvature, be ascertained. 5 - STD-BSI BS EN IS0 SbbS-ENGL 2000 m 3b24bb9 0880053 T90 EN IS0 9665:2000 Dimensions in millimetres 0 12.7 t0.013 Key 1
37、Tap 2 Brass locknut 3 Plunger Figure 1 - Detail of plunger for gelometer 7.2.5 Gel-testing instrument (penetrometer), that enables the plunger to be brought just into contact with the surface of the gel and then measures the force required to depress it vertically to a depth of 4 mm f 0,Ol mm, eithe
38、r at a constant rate of loading not exceeding 40 g/s or at a constant rate of penetration not exceeding 0,8 mds. (See annex A for details of suitable instruments.) 7.2.6 Balance, capable of weighing to the nearest 0,Ol g. 7.3 Dissolving the sample Weigh out, to the nearest 0,Ol g, 15 g of the test s
39、ample (see clause 5), and dissolve this test portion in 105 ml o water in the wide-neck bottle (7.2.1) in the manner specified in 5.3, closing the bottle with the stopper. To prevent caking, swirl the bottle vigorously to wet the glue completely. At this stage, take care not to build up more froth b
40、y excessive agitation than will collapse before the bottle is inserted in the bath (7.2.2) maintained at 65 OC f 1 OC. Particular care is necessary to see that the glue is all dissolved and that the solution is homogeneous. Place a finger over the hole in the stopper and invert the bottle several ti
41、mes to mix in the water that has condensed on the walls of the bottle and the under-side of the stopper. 7.4 Chilling the solution To prevent cracking, allow the bottle to cool for 15 min at room temperature, and then place in the enclosed thermostatic bath (7.2.3), maintained at 10 “C f Oll OC, for
42、 not less than 16 h and not more than 18 h. Ensure that the platform of the thermostatic bath is horizontal and that the bottle stands evenly on it. 7.5 Procedure for determining gel strength NOTE - See annex A for detailed instructions for particular instruments. 7.5.1 It is essential that the inst
43、rument stands perfectly level on a rigid support, that the plunger face is parallel to the gel surface, and that the direction of plunger travel is perpendicular to the gel surface. 6 STD-BSI BS EN IS0 9bb5-ENCL 2000 = Lb24bb9 0880052 927 EN IS0 9665:2000 7.5.2 Place the test bottle containing the g
44、el on the platform of the penetrometer so that the centre of the gel is underneath the plunger. Proceed with the sequence of operations required for the particular type of instrument in use and record the force required to depress the plunger 4 mm into the gel. If the gel strength is above 400 g, re
45、peat the test using a solution prepared by dissolving 7,5 g of the test sample in 105 ml of water to give a solution concentration of 6,67 %. 7.6 Expression of results Express the result as the force, in newtons, required to depress the plunger 4 mm into the gel. NOTE - In some instruments, the forc
46、e is applied by the addition of weights to a container attached to a counter-balanced plunger, and it has been customary with such instruments to quote the gel strength as “grams Bloom”, this being numerically equal to the mass of the container plus the added weights. To enable comparison of current
47、 results with earlier records, it should be noted that 1 N is numerically equal to 101,972 “grams Bloom”. 7.7 Test report The test report shall include the following information: a) a reference to this International Standard; b) all details necessary for the complete identification of the glue teste
48、d; c) the number of containers sampled and the mass of glue taken from each container; d) the result of the test, the concentration of the glue solution and any circumstances which may have affected the results; e) the method and instrument used. 7.8 Validation of the test method The following three
49、 criteria shall be satisfied in order to validate the test method: The diameter of the gelometer plunger and the radius of curvature of its lower circular edge shall conform to the dimensions given in figure 1. NOTE 1 A profilometer is a satisfactory instrument for measuring the radius of curvature. The gelometer used shall be calibrated using a device consisting of a strip of metal, supported near each end, which offers a pre-determined resistance, simulating that of the surface of a gel being tested. NOTE 2 This device is sometimes known as a “dummy Bloom” device and can usu
