GB/T 27844-2011 Dissolution/precipitation characteristics of chemical polymers in water GB/T27844-2011 Standard compression package decompression password: www.bzxz.net
This standard specifies the determination method of the dissolution and precipitation characteristics of polymers in water. This standard is applicable to the determination of the dissolution and precipitation characteristics of polymers in water. This standard is not applicable to liquid polymers and polymers that react with water under these test conditions. When the method in this standard is not applicable or cannot be used, the dissolution/precipitation characteristics should be studied by other methods. In this case, the details of the method adopted and the reasons for its use shall be given.
This standard was drafted in accordance with the rules given in GB/T1.1-2009.
This standard has the same technical content as the OECD Guide to Test Methods for Chemicals No. 120 (2000) "Solubility/Precipitation Characteristics of Polymers in Water" (English version).
This standard has been edited as follows:
———The background introduction in the original text has been deleted;
———The chapter "Normative References" has been added, in which the technical content of GB/T21845 is the same as that of OECD No. 105:1995, and the technical content of GB/T22236 is the same as that of DIN53733:1976.
This standard was proposed and managed by the National Technical Committee for the Administration of Hazardous Chemicals (SAC/TC251). The
drafting organizations of this standard are: China Institute of Inspection and Quarantine, China Chemical Economic and Technological Development Center, Jiangsu Coal Chemical Engineering Design and Research Institute Co., Ltd., and Sinochem Chemical Standardization Research Institute.
The main drafters of this standard are: Zhang Jing, Chen Huiming, Wang Xiaobing, Yang Ting, Guo Xinyu.
The following documents are indispensable for the application of this document. For all dated references, only the dated version applies to this document. For all undated references, the latest version (including all amendments) applies to this document.
GB/T21845 Test for water solubility of chemicals
GB/T22236 Inspection of plastics Crushing of plastic products for inspection

[CS 13.300;11.100
National Standard of the People's Republic of China
GB/T27844-—2011
Chemicals
Solubility/extraction behaviour of polymers in water
Chemicals-Solution/extraction behaviour of polymers in water2011-12-30 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of ChinaStandards Administration of Standardization of the People's Republic of China
Implementation on August 1, 2012
This standard was drafted in accordance with the rules given in GB/T1.1—2009. GB/T27844—2011
This standard has the same technical content as the Organization for Economic Cooperation and Development (OECD) Guidelines for Test Methods for Chemicals No. 120 (2000) Solubility/extraction behaviour of polymers in water (English version). This standard has made the following editorial changes:
The background introduction in the original text has been deleted!
A chapter called "Normative References" has been added, in which GB/T 21845 has the same technical content as OECD No. 105:1995, and GB/T22236 has the same technical content as DIY53733:1976. This standard is proposed and managed by the National Technical Committee for the Management of Hazardous Chemicals (SAC/TC 251). The drafting units of this standard are: China Institute of Inspection and Quarantine, China Chemical Economic and Technological Development Center, Jiangsu Coal Chemical Engineering Design and Research Institute Co., Ltd., and Sinochem Chemical Standardization Research Institute. The main drafters of this standard are: Zhang Jing, Chen Huiming, Wang Xiaobing, Yang Jie, Guo Xinyu, I
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1 Scope
Chemicals Dissolution/precipitation characteristics of polymers in water This standard specifies the determination method for the dissolution and precipitation characteristics of polymers in water. This standard This standard is applicable to the determination of the dissolution and precipitation characteristics of polymers in water. GB/T27844—2011
This standard is not applicable to liquid polymers and compounds that react with water under these test conditions. When the method in this standard is not applicable or cannot be used, the dissolution/precipitation characteristics should be studied by other methods. In this case, the details of the method adopted and the reasons for its use should be given. 2 Normative references
The following documents are indispensable for the reference of this document. For all references with dates, only the date is noted. The latest version of the referenced document shall apply to this document. For any undated referenced document, the latest version (including all amendments) shall apply to this document. GB/T21845 Water solubility test for chemicals
GB/T22236 Inspection of plastics - Pulverization of plastic products for inspection 3 Method Principle
The solubility/precipitation characteristics of the compound in water medium are determined by the following improved flask method (see GB/T21845). For some specific compounds, such as emulsions of polymers, before adopting this standard, There is preliminary preparation work. 4 Method description
4.1 Test equipment
The equipment used in the test includes:
a crushing device, such as a grinder that can produce a product with known particle size (see GB/T22236); a temperature-controlled swing device:
a membrane filter system;
an analytical instrument;
——-standard sieve.
4.2 Sample preparation
Grind a representative sample with appropriate equipment to reduce the particle size to 0.125 mm~0.25 mm, in order to ensure the stability of the sample, the grinding process should be cooled. Rubbery materials can be crushed at liquid nitrogen temperature (see GB/T22236). If the required particle size is still not reached, the particle size should be reduced as much as possible, and this should be reported in the test results. In the test report, the storage method of the crushed sample before the test should be stated. 4.3 Test process
4.3.1 Operation steps
Weigh 3 10g samples of the test substance and put them into 3 containers with glass stoppers respectively, and add 1000 liters of water to each. If it is proved that 1
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GB/T27844—2011
treating 10 compounds is not feasible, the maximum treatment amount and water volume for the next time should be appropriately adjusted. Cover the container stopper tightly and shake it continuously at 20 degrees. Stirring or stirring should be carried out at a constant temperature. After 24 hours, the contents of each container are centrifuged or filtered and the concentration of the compound in the clear aqueous phase is determined by an appropriate analytical method. If no suitable analytical method is available, the total solubility and precipitation rate can be estimated from the dry weight of the filter residue or centrifugal precipitate.
It is necessary to quantitatively distinguish between impurities and additives and between various low molecular weight matrix substances. In the gravimetric determination, a blank test without the test substance should be carried out in order to calculate the residues that appear during the test. The dissolution/precipitation characteristics of the compound under the conditions of water temperature 20°C, pH value 2 and pH value 9 and water temperature 37°C and pH value 7 can be determined by the same method. The pH value can be controlled by adding a suitable buffer solution or an appropriate acid or base (such as hydrochloric acid, acetic acid, analytical grade sodium hydroxide, analytical grade potassium hydroxide or ammonia). Depending on the analytical method used, 1~2 tests should be carried out. When there is a method to directly analyze the composition of the polymer in the aqueous phase, it is sufficient to do the above test. However, when no reliable method is available and the solubility/precipitation characteristics of the polymer are limited to the indirect determination of the total organic carbon (TOC) in the precipitate from the aqueous solution, an additional test should be performed. The additional test should be performed three times with less than 10 times the sample of the polymer used in the above test (see 4.3.1) and an equal amount of water. 4.3.2 Analysis
4.3.2.1 Test with one sample
When appropriate analytical methods are available, the polymer components in the aqueous phase can be directly analyzed. Alternatively, the solubility/precipitation rate of the polymer components can be analyzed indirectly by determining the total content of the soluble components or by considering the correction of non-specific polymer components. Aqueous phase analysis of total affinity species can be performed by highly sensitive methods including, but not limited to, digestion with persulfate or dichromate to generate carbon dioxide followed by estimation of TOC by infrared spectroscopy (IR) or chemical analysis: atomic absorption spectroscopy (AAS) or inductively coupled plasma emission spectroscopy (ICP) for silicon or metals in the presence of compounds: ultraviolet absorption amplification (UV) or fluorescence spectrophotometry for aromatic compounds; liquid chromatography-mass spectrometry (LC-MS) for low molecular weight samples. Alternatively, the aqueous extract can be evaporated under vacuum and dried, followed by analysis of the residue by spectroscopic methods (IR, UV, etc.) or AAS/ICP. If these aqueous phase analyses are not feasible, extraction should be performed with a water-immiscible organic solvent (e.g., chlorinated hydrocarbons). The organic solvent is evaporated and the residue analyzed by IR, UV, AAS/ICP, etc. to determine the content of the compound. Any components identified as impurities or additives should be subtracted to determine the degree of solubility/precipitation of the compound itself. When these substances are present in relatively large amounts, it may be necessary to analyze the residue using high performance phase chromatography (HPLC) or gas chromatography (GC) to distinguish impurities from monomers and monomer derivatives and thus determine the true composition. In some cases, it is sufficient to simply evaporate the organic solvent to dryness and weigh the dry residue. 4.3.2.2 Analyze the TOC of all aqueous precipitates using two different sample size tests.
Determine the insoluble/non-precipitated portion of the sample by gravimetric analysis. If the residue of the compound in each container is still attached to the container wall after centrifugation or filtration, the container should be rinsed with the filtrate until all visible residue in the container is washed off. Then centrifuge or filter all the filtrates. The residue attached to the filter or centrifuge tube is vacuum dried at 40 and weighed. The drying should be continued until constant weight is reached. 5 Data processing and test report
5.1 Tests with one sampleWww.bzxZ.net
The results of each measurement of the three containers and the average value should be given in units of mass per unit volume of solution (e.g. m/L.) or mass per unit volume of polymer sample (e.g. mg/g). In addition, the sample loss (calculated by dividing the mass of the solute by the mass of the initial sample) should be given, and the relative standard deviation (RSD) should be calculated. The individual data of all substances (polymers and important additives, etc.) and the data of individual compounds (excluding the influence of additives) should be given. 5.2 Tests with two different sizes of samples For the TOC values ​​of the precipitates in the aqueous solution of the two groups of three tests and the average value of each test, express them in mg/L and mg/g. Note: mg/l.;Mass of free liquid per unit volume (in C); mg/g: mass of original sample per unit mass (in C). If there is no difference between high and low sample/water ratios, it means that all precipitable components have been precipitated. In this case, direct analysis is not necessary. The respective amount of residue should be given, expressed as a percentage of the initial content of the sample, and the average value should be calculated for each test. The difference between 100% and the determined percentage gives the percentage of dissolved/precipitated material in the initial sample. 5.3 Test report
5.3.1 Test substance
All available information on the test substance (characteristics, additives, impurities, low molecular weight fraction). 5.3.2 Test conditions
The test report should contain the following test conditions: description of the test procedure and test conditions;
- description of the analytical and determination methods.
5.3.3 Test results
The test report should contain the following test results: Solubility/precipitation rate results (mg/L): Individual and average values ​​of precipitation tests in different solutions, polymer decomposition parts and materials, additives, etc.:
Solubility/precipitation rate results of polymer (mg/g) - TUC value of water extract, mass of dissolved matter and calculated percentage (such as nest determination); pH value of each sample
- Blank test value;
- If necessary, there should be information on the instability of the test material during the test and analysis process; - All important information for interpreting the results. TTTKAONTKACA
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