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Basic dataStandard ID: GB/T 9567-2016 (GB/T9567-2016)Description (Translated English): Melamine for industrial use Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: G17 Classification of International Standard: 71.080.30 Word Count Estimation: 14,118 Date of Issue: 1988-06-28 Date of Implementation: 2017-09-01 Older Standard (superseded by this standard): GB/T 9567-1997 Regulation (derived from): National Standard Notice No. 14 of 2016 Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China GB/T 9567-2016: Melamine for industrial use---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.Melamine for industrial use ICS 71.080.30 G17 National Standards of People's Republic of China Replace GB/T 9567-1997 Industrial Melamine 2016-08-29 released 2017-09-01 Implementation General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Issued by China National Standardization Administration ForewordThis standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 9567-1997 "Industrial Melamine", compared with GB/T 9567-1997, the main technical content changes as follows. ---The "first-class product" in the technical requirements is changed to "qualified product", and the index remains unchanged; the index of "melamine" for superior product is changed from "≥99.8%" "≥99.5%" (see Chapter 3, Chapter 3 of the.1997 edition); ---Determine the "picric acid method" as the arbitration method for the determination of melamine content (see 4.3.1,.1997 edition 5.4.1); ---Added the Karl Fischer method to determine moisture, and confirmed it as the arbitration method (see 4.4.2); ---Revised the "Test Method for Dissolution of Formaldehyde in Water" (see 4.7, 5.8 in the.1997 edition); ---Combine part of the "Sampling" chapter and "Test Methods" into the "Inspection Rules" chapter (see Chapter 5,.1997 edition Chapter 4 and 5.2); ---Added the requirement of "Strictly used in food and related industries" in Chapter 6 (see 6.1). This standard was proposed by the China Petroleum and Chemical Industry Federation. This standard is under the jurisdiction of the Organic Chemical Branch of the National Chemical Standardization Technical Committee (SAC/TC63/SC2). Drafting organizations of this standard. China Petroleum & Chemical Corporation Beijing Research Institute of Chemical Industry, Shandong Hualu Hengsheng Chemical Co., Ltd., Sichuan Golden Elephant Serui Chemical Co., Ltd., Luxi Chemical Group Co., Ltd. Participated in the drafting of this standard. Sichuan Chemical Co., Ltd., Chengdu Yulong Chemical Co., Ltd. The main drafters of this standard. Lei Weiping, Liu Zhongfa, Fan Yanru, Huang Yu, Zhang Yanli, Liu Chaohui, Zhang Wen, Hu Wenhong, Tang Yin, Chen Duanyang, Zhao Xiuying. This standard was first issued in 1988 and was revised for the first time in.1997.This is the second revision. Industrial Melamine1 ScopeThis standard specifies the technical requirements, test methods, inspection rules, signs, packaging, transportation and storage of industrial melamine. This standard applies to industrial melamine made from urea. Structural formula. Molecular formula. C3H6N6 Relative molecular mass. 126.12 (according to the.2011 international relative atomic mass)2 Normative referencesThe following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. Preparation of preparations and products used in GB/T 603 chemical reagent test method GB/T 6283-2008 Determination of water content in chemical products Karl Fischer method (general method) GB/T 6678 General Rules for Sampling of Chemical Products GB/T 6679 General rules for solid chemical sampling GB/T 6682 Analytical laboratory water specifications and test methods GB/T 8170 Numerical rounding rules and the expression and determination of limit values GB/T 8946-2013 General technical requirements for plastic woven bags GB/T 10454 FIBC3 requirements3.1 Appearance. white or light yellow solid powder without visible impurities. 3.2 Melamine for industrial use should meet the technical indicators shown in Table 1.4 Test methodWarning. Some processes specified in the test method may lead to dangerous situations, and the operator should take appropriate safety and protective measures. 4.1 General rules Unless otherwise specified, only use reagents confirmed to be analytically pure and the tertiary water specified in GB/T 6682 in the analysis. Preparations and products used in the analysis, unless other requirements are specified, are prepared in accordance with the provisions of GB/T 603. 4.2 Determination of appearance Take an appropriate amount of sample in a watch glass or sample bag and observe it visually under natural light or fluorescent light. 4.3 Determination of melamine content 4.3.1 Picric Acid Method (Arbitration Law) 4.3.1.1 Method summary Add water to the sample, heat it to dissolve, add picric acid solution, weigh the mass of the picric acid melamine precipitated, that is, the melamine is measured Amine purity content. 4.3.1.2 Reagents and solutions 4.3.1.2.1 Sulfuric acid solution. 1,200. 4.3.1.2.2 Phenolphthalein indicator solution. 10g/L. 4.3.1.2.3 Picric acid solution. 10g/L. 4.3.1.2.4 Saturated melamine picric acid solution. Weigh 1g sample, place it in a 500mL Erlenmeyer flask, add 400mL water and heat to dissolve it. solution. After cooling, add 3 drops of phenolphthalein indicator solution. If it develops color, add sulfuric acid solution until the color of the solution disappears; if there are insoluble materials, filter, water wash. Combine the filtrate with the washing solution to make the total volume 500mL and transfer it into a.2000mL beaker; heat this solution to 80°C in a water bath, In addition, add 500mL picric acid solution heated to 80℃, after cooling to room temperature, keep it below 15℃ for about 8h; filter with glass sand Filter, wash with 50mL of water, dry the washed precipitate at 100℃~105℃ for 2h, and cool it for later use. Take the sediment (or sub The precipitate of picric acid melamine collected after precipitation) 3g~4g, add 2L of water, boil for 5min, filter the discarded liquid after cooling, and take the precipitate to dry For use, the precipitate is the melamine picric acid precipitate. Take 1g of melamine picric acid precipitate, add 2L of water, heat to dissolve and let stand Store. The saturated solution of melamine picric acid can be filtered at any time to make it consistent with the washing temperature. 4.3.1.3 Apparatus and equipment 4.3.1.3.1 General laboratory instruments and equipment. 4.3.1.3.2 Glass sand filter (crucible shape). G4. 4.3.1.4 Analysis steps First weigh 1g of the sample (accurate to 0.0002g), place it in a 500mL Erlenmeyer flask, then add 400mL of water and heat to dissolve. cool down After that, add 3 drops of phenolphthalein indicator solution. If the color develops, add sulfuric acid solution until the color of the solution disappears; if there are insoluble matter, filter and wash with water. Filter Combine the liquid and lotion, transfer to a 500mL volumetric flask, add water to the mark, shake carefully to mix, and accurately absorb 100mL of this solution and place it in In a 500mL beaker; heat this solution in a water bath to 80℃, add another 100mL picric acid solution heated to 80℃, and cool to After room temperature, keep it below 15°C for about 8 hours; filter with a glass sand filter that has a constant weight, and then use about 100 mL of melamine picric acid Wash with saturated solution, then wash with 10mL of water; After drying the glass sand filter for 2h at 100℃~105℃, place it in a desiccator to cool, Weigh (accurate to 0.0002g) to obtain the mass of the precipitate. 4.3.1.5 Calculation of analysis results The mass fraction w1 of melamine is calculated according to formula (1). Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.2%. 4.3.2 Sublimation method 4.3.2.1 Method summary In the sublimation device, the sample is heated under negative pressure, after the melamine is completely sublimated, the amount of residue is weighed, that is, the melamine is measured purity. 4.3.2.2 Test device The structure of the decompression sublimation device of the sample is shown in Figure 1, and the following conditions must be met. a) The material of the sample container is platinum, glass, magnet, etc., and its shape is disc or tube, so that the inside sample is easy to sublime, and the pressure is reduced. No splashing during the sublimation process; b) The decompression sublimation device should use a heating device with a temperature control internal temperature of (305±10) ℃ and an internal pressure of below 4.00kPa Set and vacuum device. 4.3.2.3 Analysis steps Weigh about 2g of the sample (accurate to 0.0002g) and place it in a pre-dried sample container of known mass; put the sample container into In the decompression sublimation device, after it is completely sealed, turn on the vacuum device to slowly attract, and reduce the pressure to 0.67kPa~4.00kPa; about Adjust the temperature in the device to (305±10)℃ within 20min; then, under the pressure of 0.67kPa~4.00kPa, temperature (305±10)℃ Continue to sublime under the sample, and the sublimation ends after 1h; stop heating and suction, and let the pressure in the device return to normal pressure slowly, then take out the sample volume Device. After cooling to room temperature in a desiccator, weigh the mass of the sample container (accurate to 0.0002g) to obtain the residual amount. 4.4.1.2 Instruments and equipment 4.4.1.2.1 Flat bottom weighing bottle 50mm×30mm. 4.4.1.2.2 Constant temperature drying oven. 4.4.1.3 Analysis steps Spread about 5g of the sample evenly in a pre-dried flat-bottomed weighing bottle of known mass, cover the cap, and weigh to the nearest 0.0002g; Open the lid, place the weighing bottle and the lid in a drying box whose temperature is adjusted to (105±1)℃ for 2h; put the weighing bottle and the lid in a glass desiccator After the lid is allowed to cool to room temperature, weigh it and determine its reduction. 4.4.1.4 Result calculation The mass fraction of water w2 is calculated according to formula (3). Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.02%. 4.4.2 Karl Fischer Law (Arbitration Law) 4.4.2.1 Method summary The free water in the sample reacts quantitatively with the Karl Fischer reagent of known water titration. 4.4.2.2 Reagents and solutions 4.4.2.2.1 5A molecular sieve. 3mm~5mm in diameter, used as a desiccant. Before use, calcinate at 500℃ for 2h, and install molecular sieve inside The used molecular sieve can be washed with water, dried, roasted and regenerated for use after cooling in the dryer. 4.4.2.2.2 Methanol. water content ≤0.05%, if the reagent water content exceeds 0.05%, add about 50g of 5A molecular sieve to 500mL methanol, Put the stopper on the bottle, let it stand overnight, and draw the supernatant for use. 4.4.2.2.3 Anhydrous ethanol. dehydrated. 4.4.2.2.4 Karl Fischer reagent. Note. Karl Fischer modified reagent without pyridine can also be used, but in arbitration, only pyridine-containing reagents can be used. 4.4.2.3 Instruments and equipment 4.4.2.3.1 Karl Fischer Moisture Analyzer. According to GB/T 6283-2008 Appendix C configuration or equivalent Karl Fischer instrument. 4.4.2.3.2 Centrifuge. 4.4.2.3.3 Syringe. 4.4.2.4 Analysis steps 4.4.2.4.1 Calibration of Karl Fischer reagent According to GB/T 6283 direct coulometric titration method, use sodium tartrate dihydrate or water to calibrate the water titration of Karl Fischer reagent Degree T. 4.4.2.4.2 Determination In a 250mL iodine measuring bottle, weigh 20g~30g of melamine sample, accurate to 0.001g, cover the bottle stopper, and inject it with a syringe 100.0mL methanol, shake or shake for a few minutes, let stand for 5 minutes, then shake or shake for a few minutes, after the sample settles slightly, take the supernatant 10mL is analyzed according to the procedures specified in GB/T 6283 direct coulometric titration method. At the same time, analyze the moisture content in methanol. 4.4.2.5 Result calculation The mass fraction of water w2 is calculated according to formula (4). Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.02%. 4.5 Determination of pH 4.5.1 Method summary Add water to the sample, boil it and then quench it, and measure the pH of the supernatant liquid. 4.5.2 Apparatus and equipment Glass electrode pH meter. The accuracy is 0.1pH unit. 4.5.3 Analysis steps Weigh 5.0g of the sample into a.200mL tall beaker, and add 100mL of pre-boiled water to remove carbon dioxide (pH6.5~7.0) Boil for 5min; in order to avoid the influence of carbon dioxide in the air, quench to 20.0℃ within 10min, and immediately determine the pH of the supernatant liquid. 4.6 Determination of Ash 4.6.1 Method summary The sample is placed in a high-temperature furnace for high-temperature ashing, and the residual amount is weighed to obtain the ash content. 4.6.2 Apparatus and equipment 4.6.2.1 Platinum, porcelain crucible or quartz crucible. 4.6.2.2 High temperature furnace. 4.6.3 Analysis steps Weigh more than 10g sample (the sampling amount varies with the ash content), accurate to 0.02g, and place it in a pre-dried and known mass crucible In the crucible; place the crucible on an electric hot plate whose temperature is pre-adjusted to 400℃~500℃ to make most of the samples volatilize and carbonize; then, put Put it into a high temperature furnace adjusted to (750±50)℃ for ashing, take it out after 1h; take out the crucible and place it in a glass desiccator, and cool to room temperature After that, weigh out the residual amount, accurate to 0.0002g, and obtain the ash content. 4.6.4 Result calculation The mass fraction w3 of ash content is calculated according to formula (5). Take the arithmetic mean of the two parallel determination results as the determination result, and the difference between the two parallel determination results shall not exceed 0.01%. 4.7 Formaldehyde water dissolution test 4.7.1 Method summary The neutralized aqueous formaldehyde solution was added to the sample, and the turbidity and color were measured after heating and dissolving. 4.7.2 Apparatus and equipment 4.7.2.1 Formaldehyde water dissolution test device. as shown in Figure 2. 4.7.2.2 Air cooling tube. a glass tube with an inner diameter of 6mm and a length of 500mm. 4.7.2.3 Thermometer. 4.7.2.4 Glass electrode pH meter. same as 4.5.2. 4.7.2.5 Electromagnetic stirrer. 4.7.3 Reagents and solutions 4.7.3.1 Sodium hydroxide solution. 4g/L. 4.7.3.2 Formaldehyde solution. 37%~40%. 4.7.4 Analysis steps On a tray balance, weigh 20g of the sample and place it in a.200mL conical flask; add 40mL to adjust the pH with sodium hydroxide solution in advance. Make it into 8.3±0.2 formaldehyde aqueous solution and dilute to 50mL with water; install the air cooling tube and thermometer in a 100mL conical flask 上; Heat while stirring in a water bath; Dissolve within 10 minutes after reaching 80℃, and immediately dissolve the sample according to the provisions of Appendix A Determination of liquid turbidity; also in accordance with the provisions of Appendix A, determine the chromaticity of the sample solution, expressed in Hazen units. Figure 2 Test device for dissolution of formaldehyde in water5 Inspection rules5.1 All items in Chapter 3 are factory inspection items. 5.2 Under the conditions of the same raw materials and process conditions, products of the same quality are grouped together, or grouped according to the production cycle. 5.3 Sampling should be carried out in accordance with the relevant regulations of GB/T 6678 and GB/T 6679.Mix the sampled products and divide them into two clean, dry In the ground glass bottle, seal, label, and indicate the product name, batch number or production date, sampling date, product grade, and name of the sampler Wait. One bottle is for inspection, and the other bottle is sealed and kept as a sample for future reference. The retention period is half a year. 5.4 The judgment of the test result shall be carried out by the comparison method of GB/T 8170 rounding value. If one of the test results does not meet the requirements of this standard When required, samples should be taken from twice the amount of packaging for re-inspection. Even if only one index does not meet the requirements of this standard, the re-inspection result The entire batch of products is unqualified. 6 Marking, packaging, transportation and storage 6.1 Logo 6.1.1 The melamine packaging bag should have a firm and clear mark, which includes. a) Product name and trademark; b) The name and address of the manufacturer; c) Batch number or production date; d) Number of this standard; e) Product grade; f) Net content; g) The packaging bag is printed with a warning statement of "No use in food and related industries". 6.1.2 Each batch of melamine delivered should be accompanied by a quality certificate in a certain format, which includes. a) The name of the manufacturer; b) Product name; c) Batch number or production date; d) Product quality inspection results or inspection conclusions; e) Number of this standard. 6.2 Packaging Melamine uses two packaging methods. a) Double-layer packaging. the outer packaging adopts the type B plastic woven bag specified in GB/T 8946-2013; the inner packaging adopts polyethylene plastic thin Film bag, film bag tie-up, woven bag seam. The net weight of each bag is 25kg±0.1kg, 40kg±0.2kg. b) Container bag packaging. flexible container bag, its size, performance and inspection method should meet the relevant regulations of GB/T 10454, According to user needs, the net weight of each bag is 250kg±0.5kg, 500kg±1.0kg, 1000kg±2.0kg. 6.3 Transportation Melamine should be packaged intact, protected from rain and moisture during transportation. 6.4 Storage Melamine should be stored in a clean, dry and ventilated environment.Appendix A(Normative appendix) Determination of Turbidity and Color in Formaldehyde Water Dissolution Test A.1 Determination of turbidity A.1.1 Method summary The turbidity value was measured by visually observing the turbidity of the sample and comparing it with the kaolin standard liquid phase. Measuring range. 1 degree (kaolin) ~ 10 degree (high Ridge). A.1.2 Reagents and solutions A.1.2.1 Water. The used water is filtered with a filter with a pore size of about 0.1μm, and the filtrate after the initial.200mL is discarded. A.1.2.2 Refined kaolin. Take about 10g of white clay (kaolin) and place it in a 500mL beaker, add 300mL of water, and then add 0.2g 10 sodium diphosphate of crystal water (10 sodium pyrophosphate of crystal water). Then use a magnetic stirrer to stir vigorously for about 3 minutes to mix uniform. After mixing, move to a 1L graduated cylinder with stopper, add water to the 1L scale, close the stopper, and vigorously shake for about 1 min. Let stand at room temperature After 1h, use a siphon to draw the solution from the liquid level to 250mL and discard it, and take the solution below 500mL. Will be taken The solution is centrifuged for about 20 minutes with a centrifuge of about 3000 r/min, or filtered with a filter material with a pore size of 1 μm or less. Then the filtered kaolin was heated at 105°C~110°C for 3h. After putting it cold in a desiccator, put it in a jar for storage. A.1.2.3 Kaolin standard sol......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 9567-2016_English be delivered?Answer: Upon your order, we will start to translate GB/T 9567-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB/T 9567-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 9567-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. 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