This standard specifies the determination method of the practical solubility of water-soluble dyes in the range of 40℃～90℃ and the stability of their solutions. This method is not used to determine the absolute solubility. GB/T 3671.1-1996 Determination of solubility and solution stability of water-soluble dyes GB/T3671.1-1996 Standard download decompression password: www.bzxz.net

GB/T 3671.1-1996
This standard is based on the International Organization for Standardization ISO 105-Z07:1995 "Determination of solubility and solution stability of water-soluble dyes" and GB/T 3671---83 "Solubility of water-soluble dyes" The Determination Method "Reduced Pressure Filtration Method" has been comprehensively revised. It is equivalent to this international standard in terms of technical content and writing format.
1SO105-Z07 specifies two specifications of filter paper used. Because there is no domestic supply of the same type of filter paper, my country's filter paper quality indicators are not completely consistent with the filter paper specifications in international standards. During the drafting process of this standard, verification and comparative tests showed that satisfactory results can be achieved by using domestic rapid qualitative filter paper of certain specifications. Appendix A is a reminder appendix.
This standard will replace GB/T3671-83 from the effective date. This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shanghai Dyestuff Research Institute. The main drafters of this standard: Hu Changjian, Ling Shujiang, Su Huiping. This standard was first published on May 14, 1983. :GB/T 3671: 1-1996
ISO Preface
ISO (International Organization for Standardization) is a world-wide joint organization that includes national standardization agencies (ISO member groups) of various countries. The formulation of international standards is carried out through ISO technical committees. Each member group interested in the topics engaged in by the established technical committees has the right to send representatives to participate in the committee. Any governmental or non-governmental international organization that has contact with ISO can also participate in the work. ISO and the International Electrotechnical Commission EC work closely on relevant electrotechnical standards. The draft international standard adopted by the technical committee will be approved as an international standard before it is approved. It should be distributed to all member groups for voting. At least 75% of the member groups' voting fees can be approved before the international standard ISO105-Z07 is formulated by ISO/TC38 Textile Technical Committee and SC1 Textile Color Fastness and Dye Testing Sub-Technical Committee.
IS0105 published from 1978 to 1985 is divided into thirteen parts. Each part is designated with a letter (such as \Part A\) and the date of publication. Each part includes several chapters, and each section specifies its own Alphabetical and two-digit designations (e.g. "Section A01"). These sections are republished in separate documents, each of which is also called a "Part", but retains their original alphabetical nomenclature. A complete list of this section is given in ISO 105A01
Appendix A of this standard is for reference only.
1 range
Guohao Standard of the People's Republic of China
Determination of application solubility and solution stability of water-soluble dyesGB/T 3671. 1— 1996 | |tt | This method is used to determine the degree of dissolution and its stability. This method is not used to determine absolute solubility.
Note: Appendix A lists several factors that may affect the test results, 2 cited standards
The provisions contained in the following standards constitute provisions of this standard by being quoted in this standard . At the time of publication of this standard, the versions indicated were valid. All standards are subject to revision and parties using this standard should explore the possibility of using the latest version of the standard listed below. GB/T6682-92 Analytical Laboratory Water Specifications and Test Methods (eqvISO3696:1987) ZBN64002-87 Laboratory Glass Apparatus - Neck Flask 3 Principles
At the specified temperature, prepare a set including a solubility limit at The solution of the dye to be tested with a known concentration is then suction-filtered with filter paper using a heated Buchner funnel at this temperature, and the solubility limit is determined by visually inspecting the residue on the filter paper and measuring the filtration time.
The solubility of dyes is generally measured at 90. For certain types of dyes, it is measured at a lower temperature. Generally, the test temperature is selected according to the manufacturer's recommendations. The temperature must be clearly stated in the test report (such as 90°C solubility or 60°C solubility, etc.). The solution stability of the dye is measured by storing the bath solution for 2 hours. If necessary, the solution is cooled and evaluated before filtration. The dissolution temperature and storage temperature must be indicated in the test report (for example: the solution is stable at 90℃/60℃ property or 60C/60℃ solution stability, etc.). 4 Apparatus and Reagents
4.1 Erlenmeyer flask
Wide-mouth Erlenmeyer flask with a capacity of 500mL.
4.2 Heating bath
Constant temperature controlled heating bath with electromagnetic stirrer, stirring rod length 40 nm, diameter 6 mm, stirring speed 500~600 1/min4.3 water bath||tt| |A water bath that can adjust the temperature to the storage temperature (such as 60℃, 30℃, 25℃). 4.4 Buchner funnel
A heated Buchner funnel made of glass, stainless steel or porcelain, with an inner diameter of 72mm, a volume of not less than 200ml, and a number of holes greater than 100, evenly distributed. The total area of ​​the holes is not less than 200: mm2, 4.5 constant temperature control device
National Technical Supervision 1996-08-22 batch
1997-03-01 implementation
GB/T 3671. 11996
With The thermostatic control device of the circulation pump is used to adjust the temperature of the Buchner funnel. 4.6 Vacuum device
4. 6. 1 Suction filter bottle with a volume of 1~2 L. 4.6.2 Piston pump or membrane pump
A piston pump or membrane pump that can produce high vacuum, with a vacuum of at least 50kPa. 4.6-3 The pressure regulating device used to adjust and maintain the specified vacuum degree should preferably be connected to a vacuum gauge. 4.7 Stopwatch
is used to filter the remaining time.
4.8 rapid qualitative filter paper
The diameter is 70mm±2mm.
Note, the filter paper should meet the following requirements. Under 3kPa vacuum, the time for 200mL of 85℃~95C water to pass through the double-layer paper should be 57s. The type and manufacturer of the filter paper used will be indicated in the test report. name. 4.9 Water
The water used as dye solvent should comply with the provisions of Grade 3 water in GB/T6682-92. Generally, 200 mL of water is used for dissolution. If more water is added to the solution, this addition must be noted in the report together with the solubility value of the dye.
Note, volume changes due to temperature or volume changes due to the addition of dye can be ignored. 5 Preparation of solution
5.1 The concentration grade of the prepared dye solution will be selected according to the expected solubility limit of the dye. The expected solubility is between
1 g/I.~10 g/L
10 g/L~50 g/L
50g/L~100g/L||tt| |Above 100 g/L
5.Determination of degree of dissolution at 290℃
Increase the dye concentration close to the solubility limit by 1g/L
Prepare water around 60℃ that does not exceed the dissolution temperature (4.9) 200mL, first use a small amount of water to slurry a known amount of the dye to be tested, and transfer it to a conical flask. After the gold is completely wet, pour all the remaining water into the flask. Put the solution into a heating bath adjusted to 95°C (4.2) Start the electromagnetic stirrer. When the solution reaches a temperature of 95°C ± 2'°C, continue stirring at this temperature for 5 minutes (the total stirring time is about 10 minutes) . Immediately after burning, the solution is filtered (see Chapter 6) to determine the solubility of the dye at 90 °F.
Repeat this procedure for each concentration of the dye being tested. 5.3 Determination of solution below 90℃
It is recommended to prepare a 200 mL portion of water with the required dissolution temperature (4.9), mix a known amount of the dye to be tested, and transfer it to a wide-mouth cone In the flask, after it is completely moistened, pour the remaining water into the flask completely. Put the solution into a heating bath adjusted to the dissolution temperature, stir for 10 minutes, and then filter (see Chapter 6). Repeat this procedure for each level of dye to be removed. 5.4 Determination of solution stability at the required temperature (such as 60°C, 30°C, or 25°C). Adjust the Erlenmeyer flask containing the solution prepared according to 5.1 or 5.2 to the required temperature (see 4.3) in a water bath, and filter after 2 hours. Before filtering, shake the flask to mix the solution evenly. 6 Filtration of the solution
In order to avoid the influence of sudden temperature changes, the device for filtering hot solutions must be heated to the same temperature as the test solution. It is most ideal to use a jacketed Büchner funnel GB/T 3671.1-1996 Www.bzxZ.net
, but satisfactory results can also be obtained by using a preheated funnel. Immerse the funnel in a water bath or place it in an oven, or let water preheated to the test temperature flow through the filtration device before the test. When the following method (preheating method) is used, the amount of water used for preheating is determined by being able to heat the filter funnel to the same temperature, and has nothing to do with the geometric shape of the device and the surrounding conditions. In various cases where preheating is used, it is more important than when using a jacketed funnel that the test solution must be filtered immediately after being taken out of the heating medium. 6.1 Preheat the Büchner funnel (4.4) to the test temperature and maintain this temperature throughout the filtration operation. 6.2 Before filtering, wet the double filter paper (4.8) in the Büchner funnel with at least 50 mL of water at the test temperature. 6.3 Adjust the vacuum to 3-4 kPa, which is equivalent to the vacuum of a 300-400 mm column. 6.4 Filter the dye solution prepared in accordance with 5.1.5.2 or 5.3 at the recommended temperature. Measure the filtration time with a stopwatch and visually check whether there is any residue in the flask containing the dye solution. 6.5 If the dye solution cannot be filtered out within 2 min under the specified vacuum, filter it under full vacuum, but the time shall not exceed 2 min (see 4.6.2).
6.6 After the solution has been filtered, turn on the full vacuum and dehydrate the filter paper for 1 min. 6.6.1 Allow the filter paper to dry completely at room temperature before rating. 7 Rating
7.1 Visually evaluate the dried filter paper through which the dye solutions of various known concentrations have been filtered. The concentration at which residue is visible on the filter paper is taken as the solubility limit or the solution stability limit. Sometimes, it is possible to find residues that are not easily visible by gently rubbing the filter paper with the fingertips. 7.2 Filtration time can also be used as a basis for further rating. When the filtration time increases with the increase of dye concentration, it means that the solubility limit has been exceeded, or that the solution cannot be stable for a long time. 8 Test report
The test report should include The following contents:
a) State the number and year of this standard:
b) Full name of the dye to be tested:
c) Type of filter paper used and name of the manufacturer; d) Solubility limit and dissolution temperature of the dye expressed in g/L: e) Solution stability expressed in g/L, including dissolution temperature and storage temperature; f) Corresponding filtration time (see 7.2);
g) Special circumstances during the test or assessment process: h)) Differences from this method (for example, the amount of solvent is not 200 mL, etc.). GB/T 3671.1-1996
Appendix A
(Suggestive Appendix)
Factors affecting the results
For many years, the above test method has obtained good test results, but it should be pointed out that if the test conditions are slightly different from those specified in this method, very different test results will be obtained. For example, the following circumstances will affect the results. a) Using other German paper of different specifications. The choice of filter paper must be considered comprehensively based on permeability and actual conditions. \b) Other dissolution temperatures are used. Many dyes can be well dissolved even at temperatures significantly lower than 90°C or a given temperature. Some dyes can be well dissolved at 90°C, but are difficult to dissolve at 85°C. c) Other storage temperatures and storage times are used. d) When water with different hardness or electrolytes is used,
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