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Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative. This standard is drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 4649-2008 Ethylene glycol for industrial use - Specification. The following main changes have been made with respect to GB/T 4649-2008: ——Description of ethylene glycol production process is deleted (see Clause 1; Clause 1 of Edition 2008); ——Technical requirements for acceptable products are deleted (see Table 1; Table 1 of Edition 2008); ——"superior products" are modified to "polyester grade", and "first-class products" to "industrial grade" (see Table 1; Table 1 of Edition 2008); ——The appearance requirements of polyester grade and industrial grade products are changed from "colorless, transparent and free of mechanical impurities" to "transparent liquid and free of mechanical impurities" (see Table 1; Table 1 of Edition 2008); ——The content index of polyester grade ethylene glycol is changed from “≥99.8%” to “≥99.9%” and that of diethylene glycol is changed from “≤0.10%” to “≤0.050%”; the content of diethylene glycol in industrial grade ethylene glycol is changed from “≤0.80%” to “≤0.600%”; the water content index is changed from “≤0.10%” to “≤0.08%” (see Table 1; Table 1 of Edition 2008); ——Items including 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol and ethylene carbonate are added, with the index of "report" (see Table 1; Table 1 of Edition 2008); ——Polyester grade UV transmittance is increased by 250nm, with the index of "report" (see Table 1; Table 1 of Edition 2008); ——Chloride ion item and its test methods are added under the polyester grade, with the index of "≤0.5mg/kg" (see Table 1 and 4.14; 5.7 of Edition 2008); ——The measurement unit for content of acidity, iron, ash, aldehyde and other items is changed from "%"to "mg/kg" (see Table 1; Table 1 of Edition 2008); ——The requirement of test by gravimetric method is modified in case of any dispute in the visual appearance test results (see 4.3, 4.1 of Edition 2008); ——The determination method of ethylene glycol content is modified; the original equation 1 is deleted; and the determination methods for contents of 1,2-butanediol, 1,4-butanediol, 1,2-hexanediol and ethylene carbonate are added (see 4.4; 4.2 and 4.10 of Edition 2008); ——GB/T 6324.6 is added for determination of chroma and GB/T 3143 is adopted as the arbitration method; relevant contents are moved to Annex A (see 4.5 and Annex A; 4.3 of Edition 2008); ——The U-shaped vibrating tube method given in GB/T 2013-2010 is added for density determination; the content of temperature correction in the test by density bottle method is deleted, the density bottle method given in GB/T 4472 is taken as the arbitration method, and the relevant contents are moved to Annex B (see 4.6 and Annex B; 4.4 of Edition 2008); ——104C-75 thermometer conforming to GB/T 7534-2008 is added for determination of boiling range (see 4.7); ——SH/T 1055 is added for determination of water, and the method is taken as arbitration method (see 4.8; 4.6 of Edition 2008); ——"Manual method is taken as the arbitration method" is added for determination of acidity (see 4.9; 4.7 of Edition 2008); ——The sampling amount for determination of iron content is modified from "80g" to "70g" (see 4.10; 4.8 of Edition 2008); ——The analytical balance and constant weight requirements for determination of ash are modified from "sensitivity 0.1mg" to "sensitivity 0.01mg", the "porcelain crucible” is changed to "platinum crucible", and the relevant contents are moved to Annex C (see 4.11 and Annex C; 4.9 of Edition 2008); ——The starting condition of type inspection is modified (see 5.1; 5.1 of Edition 2008); ——The determination method for inspection results is changed from "full value comparison method" to "rounded-off-value comparison method" (see 5.3); ——The clause "Safety” is deleted and the relevant contents are included in the informative annex (see Annex E; Clause 7 of Edition 2008). This standard was proposed by China Petrochemical Corporation. This standard is under the jurisdiction of Subcommittee on Petrochemistry of National Technical Committee on Chemical of Standardization Administration of China (SAC/TC 63/SC 4). The previous editions of this standard are as follows: ——GB 4649-1993, GB/T 4649-2008. Ethylene glycol for industrial use Warning——This standard does not purport to address all the safety problems, if any, associated with its use. Producers must explain to users the hazards of the product, the safety and protective measures in use, and the user of this standard is obliged to take appropriate safety and health measures which are guaranteed conforming to the conditions specified in the relevant national law and regulations. 1 Scope This standard specifies the technical requirements, test methods, inspection rules, marking, labeling and accompanying documents as well as packaging, transportation and storage of ethylene glycol for industrial use. It is applicable to ethylene glycol used as the monomer for producing polyester and alkyd resin, as well as the electrolyte, antifreeze, plasticizer and solvent for electrolytic capacitors. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 2013-2010 Standard test method for density of liquid petrochemical products GB/T 3049 Chemical products for industrial use - General method for determination of iron content - 1,10-phenanthroline spectrophotometric method GB/T 3143 Color determination method of liquid chemicals (Hazen unit - Platinum-cobalt scale) GB/T 3723 Sampling of chemical products for industrial use - Safety in sampling GB/T 4472-2011 Determination of density and relative density for chemical products GB/T 6283 Chemical products - Determination of water - Karl·Fischer method (general method) GB/T 6324.6 Test method of organic chemical products - Part 6: Determination of color for liquids - Tristimulus colorimetry GB/T 6678 General principles for sampling chemical products GB/T 6680 General rules for sampling liquid chemical products GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 7531 Determination of ignition residue for organic chemical products GB/T 7534-2004 Volatile organic liquids for industrial use - Determination of boiling range GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgment of limiting values GB/T 10479 Aluminum rail tank cars GB/T 14571.1 Test method of monoethylene glycol for industrial use - Part 1: Determination of acidity - Titration method GB/T 14571.2 Test method of ethylene glycol for industrial use - Part 2: Determination of purity and impurities - Gas chromatography GB/T 14571.3 Ethylene glycol for industrial use - Determination of content of total aldehydes present - Spectrophotometric method GB/T 14571.4 Ethylene glycol for industrial use - Determination of ultraviolet transmittance - Ultraviolet spectrophotometric method GB/T 14571.5 Test method of monoethylene glycol for industrial use - Part 5: Determination of chloride ion - Ion chromatography SH/T 1053 Determination for boiling range of industrial diethylene glycol SH/T 1055 Determination of water content in industrial diethylene glycol by microcoulometric titration 3 Technical requirements See Table 1 for the technical requirements of ethylene glycol for industrial use. Table 1 Technical requirements of ethylene glycol for industrial use S.N. Item Index Polyester grade Industrial grade 1 Appearance Transparent liquid and free of mechanical impurities 2 Ethylene glycol, ω/% ≥ 99.9 99.0 3 Diethylene glycol, ω/% ≤ 0.050 0.600 4 1,4-butanediol a, ω/% Report b 5 1,2-butanediol a, ω/% Report b 6 1,2-hexanediol a, ω/% Report b 7 Ethylene carbonate a, ω/% Report b 8 Chroma (platinum-cobalt) / scale Before heating ≤ After heating with hydrochloric acid ≤ 5 20 10 — 9 Density (20℃)/(g/cm3) 1.112 8~1.113 8 1.112 5~1.114 0 10 Boiling range (at 0℃, 0.101 33MPa) Initial boiling point / ℃ ≥ Final boiling point / ℃ ≤ 196.0 199.0 195.0 200.0 11 Water content, ω/% ≤ 0.08 0.20 12 Acidity (by acetic acid) /(mg/kg) ≤ 10 30 13 Iron content / (mg/kg) ≤ 0.10 5.0 14 Ash / (mg/kg) ≤ 10 20 15 Aldehyde content (by formaldehyde) / (mg/kg) ≤ 8.0 — 16 Ultraviolet transmittance/% 220nm ≥ 250nm 275nm ≥ 350nm ≥ 75 Report b 92 99 — 17 Chloride ion /(mg/kg)≤ 0.5 — a This item is not required for ethylene oxidation/ethylene oxide hydration process. b "report" refers to the item shall be determined and the measured data shall be provided. 4 Test methods 4.1 Sampling The sampling shall be carried out in accordance with GB/T 3723, GB/T 6678 and GB/T 6680. Mix the samples uniformly and put into two clean, dry and sealable glass bottles, attach labels on each bottle to indicate the manufacturer’s name, product name, batch No., sampling date and sampling place; keep one bottle for analysis and inspection and the other for future reference. 4.2 General requirements Unless otherwise specified, only recognized analytical reagents and Grade 3 water complying with GB/T 6682 may be used during analysis. 4.3 Appearance determination Take 50mL~60mL of industrial ethylene glycol sample, place it in a clean and dry 100mL-colorimetric tube, and perform direct visual observation under the transmission of daylight or daylight lamp. In case of any dispute, take 100g±0.5g of sample and subject it to suction filtration with a No.4 glass filter crucible of constant weight at the suction filtration speed of making the filtrate drop-like, and then wash the glass filter crucible with distilled water for 4~5 times, with an amount of about 20mL each time. Next, move the glass filter crucible into an oven, dry it at 105℃±2℃ for at least 45min, take it out, cool it in a dryer for 30min, and weigh it to the nearest 0.000 1g. Dry the glass filter crucible for another 30min, take it out, cool in a dryer for 30min, and weigh it; repeat this process until the difference between two consecutive weighing does not exceed 0.000 4g. Compare with the glass filter crucible before filtration, when the increment is not more than 0.001g, it is regarded as free of mechanical impurities. 4.4 Determination of the content of ethylene glycol, diethylene glycol, 1,4-butanediol, 1,2-butanediol, 1,2-hexanediol and ethylene carbonate It shall be in accordance with GB/T 14571.2. 4.5 Determination of chroma It shall be in accordance with Annex A. 4.6 Determination of density It shall be in accordance with Annex B. 4.7 Determination of boiling range It shall be in accordance with GB/T 7534-2004. The heat source is a 500W electric furnace or gas lamp. The main thermometer is a rod-shaped glass thermometer marked with scales of 150℃ ~ 220℃ at the division of 0.1℃. The distance from the top of the bulb to the first scale line is at least 100mm. It is also allowed to use the 104C-75 thermometer recommended in Table 1 of GB/T 7534-2004. The difference between the results of the two repeated determinations shall be no more than 0.5℃ at the initial boiling point and no more than 0.4℃ at the final boiling point. It is also allowed to use the device specified in SH/T 1053 for determination. In case of any dispute on the result, it shall be subject to the arbitration of GB/T 7534-2004. 4.8 Determination of water content It shall be in accordance with SH/T 1055 or GB/T 6283. In case of any dispute on the result, it shall be subject to the arbitration of SH/T 1055. Where GB/T 6283 is adopted, the arithmetic average obtained from two repeated determinations is taken as the analysis result. When the water content is in the range of 0.02%~0.10%, the difference between the results of two repeated determinations shall not exceed 15% of the average; when the water content is more than 0.10%, the difference between the results of two repeated determinations shall not exceed 10% of the average. 4.9 Determination of acidity It shall be in accordance with GB/T 14571.1. In case of any dispute on the result, manual titration method shall be adopted as the arbitration method. 4.10 Determination of iron content It shall be in accordance with GB/T 3049. Adopt 100mL volumetric flask or 100mL colorimetric tube and 3cm (or 5cm) cuvette when plotting the standard curves and performing sample determination. The sampling mass is 70g±0.5g. The arithmetic average of the results of two parallel determinations is taken as the analysis result. When the iron content is less than or equal to 0.5mg/kg, the difference between the results of two repeated determinations shall not exceed 15% of the average; when the iron content exceeds 0.5mg/kg, the difference between the results of two repeated determinations shall not exceed 10% of the average. 4.11 Determination of ash It shall be in accordance with Annex C. 4.12 Determination of aldehyde content It shall be in accordance with GB/T 14571.3. 4.13 Determination of ultraviolet transmittance It shall be in accordance with GB/T 14571.4. 4.14 Determination of chloride ion It shall be in accordance with GB/T 14571.5 or Annex D. In case of any dispute on the result, it shall be subject to the arbitration of GB/T 14571.5. Foreword i 1 Scope 2 Normative references 3 Technical requirements 4 Test methods 5 Inspection rules 6 Marking, labeling and accompanying documents 7 Packaging, transportation and storage Annex A (Normative) Determination of chroma Annex B (Normative) Determination of density Annex C (Normative) Determination of ash Annex D (Normative) Determination of chlorine ion content Annex E (Informative) Safety ICS 71.080.60 G 16 中华人民共和国国家标准 GB/T 4649—2018 代替GB/T 4649—2008 工业用乙二醇 Ethylene glycol for industrial use 2018-05-14发布 2018-12-01实施 国家市场监督管理总局 中国国家标准化管理委员会 发布 前 言 本标准按照GB/T 1.1—2009给出的规则起草。 本标准代替GB/T 4649—2008《工业用乙二醇》。 本标准与GB/T 4649—2008相比,主要变化如下: ——删除了乙二醇生产工艺的说明(见第1章,2008年版的第1章); ——删除了合格品技术要求(见表1,2008年版的表1); ——“优等品”修改为“聚酯级”,“一等品”修改为“工业级”(见表1,2008年版的表1); ——将聚酯级和工业级产品外观要求由“无色透明无机械杂质”修改为“透明液体,无机械杂质”(见表1,2008年版的表1); ——聚酯级乙二醇含量指标由“≥99.8%”修改为“≥99.9%”,二乙二醇含量指标由“≤0.10%”修改为“≤0.050%”,工业级乙二醇中二乙二醇含量由“≤0.80%”修改为“≤0.600%”,水分含量指标由“≤0.10%”修改为“≤0.08%”(见表1,2008年版的表1); ——增加了1,2-丁二醇、1,4-丁二醇、1,2-己二醇和碳酸乙烯酯项目,指标为“报告”(见表1,2008年版的表1); ——聚酯级紫外透光率增加了250 nm,指标为“报告”(见表1,2008年版的表1); ——聚酯级增加了氯离子项目和试验方法,指标为“≤0.5 mg/kg”(见表1和4.14,2008年版的5.7); ——修改了酸度、铁、灰分、醛含量等项目的计量单位,由“%”修改为“mg/kg”(见表1,2008年版的表1); ——修改了外观目视测定结果有争议时的重量法测试要求(见4.3,2008年版的4.1); ——修改了乙二醇含量的测定方法,删除了原公式1,增加了1,2-丁二醇、1,4-丁二醇、1,2-已二醇和碳酸乙烯酯含量的测定方法(见4.4,2008年版的4.2、4.10); ——色度测定增加了GB/T 6324.6,以GB/T 3143为仲裁方法,将相关内容移入附录A(见4.5、附录A,2008年版的4.3); ——密度测定增加了GB/T 2013—2010的U型振动管法,删除了密度瓶法测试中温度校正的内容,以GB/T 4472密度瓶法为仲裁法,将相关内容移入附录B(见4.6、附录B,2008年版的4.4); ——沸程测定增加了符合GB/T 7534—2008规定的104C-75温度计(见4.7); ——水分测定增加了SH/T 1055,并以该法为仲裁法(见4.8,2008年版的4.6); ——酸度测定增加了以手动法为仲裁法的规定(见4.9,2008年版的4.7); ——修改了铁含量测定的取样量,由“80 g”修改为“70 g”(见4.10,2008年版的4.8); ——修改了灰分测定用分析天平及恒重要求,由“感量0.1 mg”修改为“感量0.01 mg”,将“瓷坩埚”修改为“铂坩埚”,将相关内容移入附录C(见4.11、附录C,2008年版的4,9); ——修改了型式检验的启动条件(见5.1,2008年版的5.1); ——修改了检验结果的判定方法,由“全数值比较法”修改为“修约值比较法”(见5.3); ——删除“安全”一章,相关内容列入资料性附录。(见附录E,2008年版的第7章)。 本标准由中国石油化工集团公司提出。 本标准由全国化学标准化技术委员会石油化学分会(SAC/TC 63/SC 4)归口。 本标准所代替标准的历次版本发布情况为: ——GB 4649—1993、GB/T 4649—2008。 工业用乙二醇 警示——本标准未指出所有可能的安全问题。生产者必须向用户说明产品的危险性,使用中的安全和防护措施,本标准的使用者有责任采取适当的安全和健康措施,并保证符合国家有关法规规定的条件。 1 范围 本标准规定了工业用乙二醇的技术要求、试验方法、检验规则、标志、标签和随行文件、包装、运输和贮存。 本标准适用于作为生产聚酯、醇酸树脂的单体,以及作为电解电容器的电解液、抗冻剂、增塑剂、溶剂等用途的乙二醇。 2规范性引用文件 下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件,仅注日期的版本适用于本文件。凡是不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。 GB/T 2013—2010液体石油化工产品密度测定法 GB/T 3049 工业用化工产品 铁含量测定的通用方法 1,10-菲啰啉分光光度法 GB/T 3143液体化学产品颜色测定法(Hazen单位——铂-钴色号) GB/T 3723 工业用化学产品采样安全通则 GB/T 4472—2011化工产品密度、相对密度的测定 GB/T 6283化工产品中水分含量的测定 卡尔·费休法(通用方法) GB/T 6324.6有机化工产品试验方法 第6部分:液体色度的测定 三刺激值比色法 GB/T 6678 化工产品采样总则 GB/T 6680 液体化工产品采样通则 GB/T 6682 分析实验室用水规格和试验方法 GB/T 7531有机化工产品灼烧残渣的测定 GB/T 7534—2004 工业用挥发性有机液体 沸程的测定 GB/T 8170—2008数值修约规则与极限数值的表示和判定 GB/T 10479铝制铁道罐车 GB/T 14571.1工业用乙二醇试验方法 第1部分:酸度的测定 滴定法 GB/T 14571.2工业用乙二醇试验方法 第2部分:纯度和杂质的测定 气相色谱法 GB/T 14571.3工业用乙二醇中醛含量的测定 分光光度法 GB/T 14571.4工业用乙二醇紫外透光率的测定 紫外分光光度法 GB/T 14571.5工业用乙二醇试验方法 第5部分:氯离子的测定 离子色谱法 SH/T 1053工业用二乙二醇沸程的测定 SH/T 1055 工业用二乙二醇中水含量的测定(微库仑滴定法) 3技术要求 工业用乙二醇的技术要求见表1。 表1工业用乙二醇的技术要求 编号 项 目 指 标 聚酯级 工业级 1 外观 透明液体,无机械杂质 2 乙二醇,w/% ≥ 99.9 99.0 3 二乙二醇,w/% ≤ 0.050 0.600 4 1,4-丁二醇a,w/% 报告b 5 1,2-丁二醇a,w/% 报告b 6 1,2-己二醇a,w/% 报告b 7 碳酸乙烯酯a,w/% 报告b 8 色度(铂-钴)/号 加热前 ≤ 加盐酸加热后 ≤ 5 20 10 — 9 密度(20℃)/(g/cm3) 1.112 8~1.113 8 1.112 5~1.114 0 10 沸程(在0℃,0.101 33 MPa) 初馏点/℃ ≥ 干点/℃ ≤ 196.0 199.0 195.0 200.0 11 水分,w/% ≤ 0.08 0.20 12 酸度(以乙酸计)/(mg/kg) ≤ 10 30 13 铁含量/(mg/kg) ≤ 0.10 5.0 14 灰分/(mg/kg) ≤ 10 20 15 醛含量(以甲醛计)/(mg/kg) ≤ 8.0 — 16 紫外透光率/% 220 nm ≥ 250 nm 275 nm ≥ 350 nm ≥ 75 报告b 92 99 — 17 氯离子/(mg/kg) ≤ 0.5 — a 乙烯氧化/环氧乙烷水合工艺对该项目不作要求。 b “报告”是指需测定并提供实测数据。 4试验方法 4.1 取样 取样应按照GB/T 3723、GB/T 6678和GB/T 6680规定进行。将所采样品充分混匀后,分装于2个清洁、干燥的可密封的玻璃瓶中,贴上标签,注明生产厂名称、产品名称、批号、取样日期和取样地点,一瓶做检验分析,另一瓶做留样备查。 4.2一般规定 除非另有说明,在分析中仅使用确认为分析纯的试剂和符合GB/T 6682的三级水。 4.3外观的测定 取50 mL~60 mL工业用乙二醇试样,置于清洁、干燥的100 mL比包管中,在目光或日光灯透射下,直接目测。 如有争议时,取100 g±0.5 g试样,用已恒重的4号玻璃滤埚抽滤,抽滤速度应控制在使滤液呈滴状,再用蒸馏水洗涤玻璃滤埚4次~5次,每次用量约20 mL。然后,将玻璃滤埚移入烘箱中,在105℃±2℃下至少干燥45 min,取出,放在干燥器中冷却30 min,进行称量,精确至0.000 1 g。再将玻璃滤埚干燥30 min,取出置于干燥器中冷却30 min,称量;如此反复,直至两次连续称量间的差值不超过0.000 4 g为止。与过滤前的玻璃滤埚相比,其增量不大于0.001 g时,认为无机械杂质。 4.4乙二醇、二乙二醇、1,4-丁二醇、1,2-丁二醇、1,2-己二醇、碳酸乙烯酯含量的测定 按GB/T 14571.2的规定进行测定。 4.5色度的测定 按附录A的规定进行测定。 4.6密度的测定 按附录B的规定进行测定。 4.7沸程的测定 按GB/T 7534—2004的规定进行。热源采用500 W电炉或煤气灯,主温度计采用标有150℃~220℃刻度值,分度值为0.1℃的棒状玻璃温度计,感温泡顶端距第一条刻度线的距离至少100 mm。也可采用GB/T 7534—2004表1推荐的104C-75温度计。两次重复测定结果的差值,初馏点应不大于0.5℃,干点应不大于0.4℃。也可采用SH/T 1053所规定的装置进行测定。结果有争议时,以GB/T 7534—2004为仲裁方法。 4.8水分的测定 按SH/T 1055的规定进行。也可采用GB/T 6283的规定进行测定。结果有争议时,以SH/T 1055为仲裁方法。 采用GB/T 6283时,取两次重复测定结果的算术平均值为分析结果。当水分在0.02%~0.10%范围时,两次重复测定结果的差值应不大于其平均值的15%;当水分大于0.10%时,两次重复测定结果的差值应不大于其平均值的10%。 4.9酸度的测定 按GB/T 14571.1的规定执行。结果有争议时,以手动滴定法为仲裁方法。 4.10铁含量的测定 按GB/T 3049的规定进行。绘制标准曲线和样品测定时,需采用100 mL容量瓶或100 mL比色管,并采用3 cm(或5 cm)比色皿。取样量为70 g±0.5 g。取两次重复测定结果的算术平均值为分析结果。当铁含量≤0.5 mg/kg时,两次重复测定结果的差值应不大于其平均值的15%;当铁含量>0.5 mg/kg时,两次重复测定结果的差值应不大于其平均值的10%。 4.11灰分的测定 按附录C的规定进行测定。 4.12醛含量的测定 按GB/T 14571.3的规定进行测定。 4.13紫外透光率的测定 按GB/T 14571.4的规定进行测定。 4.14氯离子的测定 按GB/T 14571.5或附录D的规定进行测定。结果有争议时,以GB/T 14571.5为仲裁方法。 5检验规则 5.1 检验分类 表1中的所有指标项目均为型式检验项目,除沸程、密度、铁含量、灰分、氯离子外均为出厂检验项目。当遇到下列情况之一时,应进行型式检验: a)正常生产时每隔3个月; b)关键生产工艺更新及主要设备发生更改; c) 主要原料有变化而影响产品质量; d)停产又恢复生产; e) 出厂检验结果与上次型式检验有较大差异。 5.2组批规则 同等质量的、均匀的产品为一批,可按生产周期、生产班次或产品储罐进行组批。 5.3判定规则 采用GB/T 8170—2008修约值比较法进行。检验结果全部符合本标准表1的技术要求时,则判定该批产品合格。检验结果如有任何一项指标不符合本标准的要求,则应按4.1规定重新采双倍量的样品进行检验。重新检验结果仍不符合本标准规定的相应等级品要求,则该批产品作不合格处理。 6标志、标签和随行文件 6.1工业用乙二醇产品包装容器上应有牢固的标志,其内容包括;生产厂名称、产品名称、本标准编号、批号或生产日期、净含量。 6.2乙二醇不属于危险化学品,但有一定毒性和危险性,相关安全要求参见附录E。 6.3工业用乙二醇每批出厂产品都应附有质量证明书,内容包括:生产厂名称、产品名称、等级、批号或生产日期、本标准编号等。 7包装、运输和贮存 7.1包装 工业用乙二醇应采用镀锌铁桶包装,或装入铝制或不锈钢容器的铁路槽车(铝制铁路槽车应符合GB/T 10479的要求)或船舱中。应保持容器密封。 7.2运输 工业用乙二醇在运输过程中应防漏、防火、防潮。灌装有工业用乙二醇的罐车应在干燥氮气密封下运输。铁桶包装搬运时要轻装轻卸,防止容器损坏。 7.3贮存 工业用乙二醇为吸水性物质,应储存于阴凉、通风的仓库内。远离火种、热源。防止阳光直射。在贮存过程中应保持包装容器的密闭性。应与氧化剂、酸类物质分开存放。 采用储罐贮存工业用乙二醇时,应充入干燥氮气密封。 附录A (规范性附录) 色度的测定 A.1 试剂 盐酸:优级纯。 A,2仪器与设备 A.2.1可调电炉。 A.2.2移液管:1 mL。 A.2.3标准磨口锥形瓶:250 mL。 A.2.4玻璃毛细管:直径约1 mm,长约10 mm,用盐酸煮沸,然后用蒸馏水洗净,烘干。 A.2.5空气冷却装置,见图A.1。 单位为毫米 图A.1 空气冷却装置 A.3加热前色度的测定 按GB/T 3143的规定执行,采用100 mL比色管。也可采用GB/T 6324.6进行测定。结果有争议时,以GB/T 3143为仲裁方法。 A.4加盐酸加热后色度的测定 取100 mL试样置于锥形瓶中,用移液管加入盐酸1 mL,放入2根~3根玻璃毛细管,将锥形瓶与空气冷却管连接。预热电炉5 min,然后把带有冷却管的锥形瓶置于电炉上,调整电压使试液在5 min内达到沸腾,煮沸30 s。取下锥形瓶(仍带空气冷却管),冷却1 h。 色度测定同A.3。 附 录B (规范性附录) 密度的测定 B.1 密度瓶法 按GB/T 4472—2011中4.3.1规定进行,采用50 cm3密度瓶。 乙二醇产品的密度ρ,以g/cm3计,按式(B.1)计算: (B.1) 式中: m1——密度瓶质量,单位为克(g); m2——密度瓶加试样质量,单位为克(g); m3——密度瓶加水质量,单位为克(g); 0.001 2——20℃时空气密度的数值,单位为克每立方厘米(g/cm3); ρ水——20℃时水的密度的数值,单位为克每立方厘米(g/cm3)。 取两次重复测定结果的算术平均值为分析结果。两次重复测定结果的差值应不大于0.000 2 g/cm3。 B.2 U型振动管法 按GB/T 2013—2010中第6章测定。 结果有争议时,以密度瓶法为仲裁方法。 附录C (规范性附录) 灰分的测定 C.1仪器与设备 C.1.1天平:感量为0.1 g。 C.1.2分析天平;感量为0.01 mg。 C.1.3坩埚:100 mL铂坩埚。 C.2分析步骤 按GB/T 7531的规定进行测定。灼烧温度为800℃,试样量为80 g,精确到0.1 g。空坩埚和带样品灰分的坩埚称准至0.01 mg,以两次称量结果之差不大于0.05 mg为恒重。 附录D (规范性附录) 氯离子含量的测定 D.1方法原理 试样中氯离子与硝酸银反应,生成白色氯化银沉淀,然后与标准溶液进行比浊。 D.2试剂 D.2.1氯化钠:基准试剂。 D.2.2氨水溶液:1+1。 D.2.3硝酸:分析纯。 D.2.4硝酸银,5%(质量分数)水溶液:称取5 g硝酸银,溶于水,稀释至100 mL。储存于棕色瓶中。 D.2.5氯标准溶液: D.2.5.1氯标准溶液A:称取在500℃~600℃灼烧至恒重的氯化钠(D.2.1)0.164 9 g,溶于水中,移入1 000 mL容量瓶中,稀释至刻度,摇匀。此溶液每毫升含氯0.1 mg。 D.2.5.2氯标准溶液B:用移液管吸取5 mL氯标准溶液A置于100 mL容量瓶中,加水稀释至刻度,摇匀。此溶液每毫升含氯0.005 mg。 D.3仪器和设备 D.3.1恒温水浴。 D.3.2磨口比色管:25 mL。 D.4测定步骤 D.4.1 取2支磨口比色管(D.3.2),其中一支加入4.5 mL乙二醇试样,另一支加入0.5 mL氯标准溶液B。 D.4.2在上述比色管中分别加入氨水(D.2.2)1.5 mL。摇匀,在70℃~80℃恒温水浴中加热15 min,冷却后加硝酸(D.2.3)3 mL,硝酸银溶液(D.2.4)1 mL,用水稀释至刻度,摇匀后静置2 min。 D.5结果判定 将样品溶液比色管和含氯标准溶液比色管置于黑色背景上,在自然光下,自上而下观察,对试样的混浊度和含氯标准溶液的混浊度进行比较。 D.6结果报告 当试样混浊度不深于含氯标准溶液的混浊度时,结果以<0.5 mg/kg报告;当试样混浊度深于含氯标准溶液的混浊度时,结果以>0.5 mg/kg报告。 附 录E (资料性附录) 安 全 E.1 工业用乙二醇的分子式为C2H6O2,相对分子质量为62.069(按2016年国际相对原子质量),具有一定毒性,在操作区域内,空气中最大允许浓度不超过5 mg/m3。采样现场要求具有良好的通风条件,在地上或设备上的工业用乙二醇应尽量搜集,微量残余可用大量水冲洗。 E.2皮肤接触:脱去污染的衣着,用大量流动清水冲洗;眼睛接触:提起眼睑,用流动清水或生理盐水冲洗,就医;吸入:迅速脱离现场至空气新鲜处,保持呼吸道通畅。就医。 E.3消防器具:作业时应按相关规定配备各种灭火设备。灭火时应采用细雾化水、泡沫或惰性气体。 E.4泄漏应急处理:迅速撤离泄漏污染区人员至安全区,并进行隔离,严格限制出入。切断火源。建议应急处理人员戴自吸过滤式防毒面具(全面罩),穿一般作业工作服。尽可能切断泄漏源。防止流入下水道、排洪沟等限制性空间。当发生小量泄漏时,用砂土、蛭石或其他惰性材料吸收。也可以用不燃性分散剂制成的乳液刷洗,洗液稀释后放入废水系统。当发生大量泄漏时,构筑围堤或挖坑收容。用泵转移至槽车或专用收集器内,回收或运至废物处理场所处置。 |
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