标准编号:	GB/T 14190-2017
中文名称:	纤维级聚酯（PET）切片试验方法
英文名称:	Testing methods of fiber grade polyester（PET）chip
中标分类:	W50    化学纤维综合
行业分类:	GB    国家标准
ICS分类:	59.060.20 59.060.20    人造纤维 59.060.20
发布机构:	中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会
发布日期:	2017-12-29
实施日期:	2018-7-1
标准状态:	valid
替代旧标准:	GB/T 14190-2008 纤维级聚酯切片（PET）试验方法
翻译语言:	英文
文件格式:	PDF
中文字符数:	32000 字
翻译价格(元):	600.0
交付时间:	付款后 1 个工作日

Testing methods of fiber grade polyester (PET) chip WARNING — Phenol, tetrachloroethane, dichlorobenzene, o-cresol, methanol and other similar solvents used in the tests are toxic, so measures shall be taken to prevent them from contacting the skin or being inhaled; sulfuric acid, hydrochloric acid, hydrogen peroxide and other similar reagents are highly corrosive, so measures shall be taken to prevent them from contacting the skin. The operator shall take proper safety and protection measures. During operation of gas chromatography, the detector does not ignite; it is strictly forbidden to start hydrogen needle valve in case of explosion due to leakage of hydrogen. 1 Scope This standard specifies the testing methods for the analysis items of fiber grade polyester chip (PET). This standard is applicable to the PET chips made of terephthalic acid and ethylene glycol; other functional polyester may make reference to this standard. 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 601 Chemical reagent - Preparations of reference titration solutions GB/T 603 Chemical reagent - Preparations of reagent solutions for use in test methods GB/T 4146 (all parts) Textiles - Man-made fibers GB/T 6283 Chemical products - Determination of water Karl Fischer method (general method) GB/T 6678 General principles for sampling chemical products GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values ISO 3105 Glass capillary kinematic viscometers - Specifications and operating instructions 3 Terms and definitions For the purposes of this document, the terms and definitions given in GB/T 4146 (all parts) and the following apply.   3.1 bright polyester (PET) chip polyester chip (PET) not subject to matting treatment 3.2 semi-dull polyester (PET) chip polyester (PET) chip with titanium dioxide content greater than 0.20% and less than or equal to 0.50% (mass fraction) 3.3 full dull polyester (PET) chip polyester (PET) chip with titanium dioxide content greater than or equal to 1.50% (mass fraction) 3.4 agglomerate particle particle greater than or equal to 10 μm in PET chip 3.5 irregular chip polyester chips (PET) with length longer than or equal to four times that of normal chip; with thickness, width or diameter greater than or equal to twice that of normal chip; with size less than 1/4 of conventional particle (or specified size); and of irregular shape 4 General principles for testing 4.1 Sampling Laboratory sample in the batch sample is implemented according to GB/T 6678 and the specimen mass shall not be less than 0.5 kg. 4.2 General requirements For the purpose of this standard, unless otherwise specified, all the reagents and water used refer to analytical reagents and Grade 3 water specified in GB/T 6682. Unless otherwise specified, the standard volumetric solutions, preparations and products required for this standard shall be prepared according to the requirements of GB/T 601 and GB/T 603. 5 Testing methods 5.1 Testing method of intrinsic viscosity 5.1.1 Method A (capillary viscometer method) 5.1.1.1 Method principle Determine flow time of 25°C solvent and PET solution at a concentration of 0.005 g/mL, and calculate its intrinsic viscosity according to measured flow time and solution concentration of the specimen. 1B may be selected for capillary viscometer until the kinetic energy correction item of viscometer is not taken into consideration. 5.1.1.2 Apparatus and equipment 5.1.1.2.1 Thermostatic bath: the test temperature is controlled at (25.00±0.05)°C. 5.1.1.2.2 Ubbelohde viscometer: the suspended level Ubbelohde viscometer as specified in ISO 3105 (see Figure 1); model: 1B. It is also allowed to use other types of viscometers stated in ISO 3105 that shall have equal determination results with the above-said Ubbelohde viscometer. Ubbelohde viscometer shall be adopted in dispute. 5.1.1.2.3 Conical flask with stopper: 100 mL. 5.1.1.2.4 Pipette or liquid fillers: 25 mL. 5.1.1.2.5 Balance: with precision of 0.1 mg. 5.1.1.2.6 Filter: 70 μm ~ 120 μm stainless steel cloth or corresponding sand core funnel. 5.1.1.2.7 Timer: with precision of 0.01 s. 5.1.1.2.8 Heating unit: the temperature is controlled with an accuracy of 2°C. 5.1.1.2.9 Vacuum drying oven: the pressure is less than 133.3 Pa and the temperature is controlled at (105±5)°C, .

Foreword i 1 Scope 2 Normative references 3 Terms and definitions 4 General principles for testing 4.1 Sampling 4.2 General requirements 5 Testing methods 5.1 Testing method of intrinsic viscosity 5.2 Testing method of diethylene glycol 5.3 Testing method of melting point 5.4 Testing method of terminal carboxyl group 5.5 Testing method of chroma 5.6 Testing method of agglomerate particle 5.7 Testing method of moisture 5.8 Testing method of powder dust and irregular chip 5.9 Testing method of titanium dioxide content 5.10 Testing method of ash 5.11 Testing method of iron content 5.12 Test report Annex A (Informative) Numerical relationship between two test methods for the intrinsic viscosity of solvents with different ratios Annex B (Information Appendix) Recommended specification for diethylene glycol test reaction tube

纤维级聚酯(PET)切片试验方法 警示——试验方法中使用的苯酚、四氯乙烷、邻甲酚、甲醇等溶剂具有毒性，应避免接触皮肤和吸入其蒸汽；硫酸、盐酸、过氧化氢等试剂具有强腐蚀性，应避免接触皮肤。操作者应采取适当的安全和健康防护措施。操作气相色谱时，检测器不点火，严禁开启氢气针形阀，以防止氢气泄入空间引起爆炸。 1 范围 本标准规定了纤维级聚酯(PET)切片各分析项目的试验方法。 本标准适用于以对苯二甲酸、乙二醇为原料生产的纤维级聚酯(PET)切片，其他差别化、功能性聚酯也可参照使用。 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 601 化学试剂 标准滴定溶液的制备 GB／T 603 化学试剂 试验方法中所用制剂及制品的制备 GB／T 4146(所有部分) 纺织品 化学纤维 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 6678 化工产品采样总则 GB／T 6682 分析实验室用水规格和试验方法 GB／T 8170 数值修约规则与极限数值的表示和判定 ISO 3105 玻璃毛细管运动黏度计 规范和操作说明(Glass capillary kinematic viscometers—Specifications and operating instructions) 3 术语和定义 GB／T 4146(所有部分)界定的以及下列术语和定义适用于本文件。 3.1 有光聚酯(PET)切片 bright polyester(PET)chip 未进行消光处理的聚酯(PET)切片。 3.2 半消光聚酯(PET)切片 semi-dull polyester(PET)chip 二氧化钛含量大于0.20％且小于或等于0.50％(质量分数)的聚酯(PET)切片。 3.3 全消光聚酯(PET)切片 full dull polyester(PET)chip 二氧化钛含量大于或等于1.50％(质量分数)的聚酯(PET)切片。 3.4 凝集粒子 agglomerate particle 在PET切片中测定大于或等于10μm的粒子。 3.5 异状切片 irregular chip 长度大于或等于正常切片的4倍；厚度、宽度或直径大于或等于正常切片2倍；小于常规颗粒(或规定尺寸)1／4；以及非规整形状的聚酯切片(PET)。 4 试验通则 4.1 取样 批量样品中实验室样品按GB／T 6678执行，试样量不低于0.5kg。 4.2 一般规定 本标准所用试剂和水，在没有注明其他要求时，均指分析纯试剂和GB／T 6682中规定的三级水。 本标准所用标准滴定溶液、制剂与制品，在没有注明其他要求时，均按GB／T 601、GB／T 603规定制备。 5 试验方法 5.1 特性黏度的试验方法 5.1.1 方法A(毛细管黏度计法) 5.1.1.1 方法提要 测定25℃的溶剂和浓度为0.005g／mL的PET溶液的流出时间，根据测量所得的流出时间和试样的溶液浓度计算其特性黏度。毛细管黏度计选用1B，达到使黏度计的动能校正项不予考虑的要求。 5.1.1.2 仪器和设备 5.1.1.2.1 恒温浴：温度控制(25.00±0.05)℃。 5.1.1.2.2 乌氏黏度计：符合ISO 3105规定的气承液柱式乌氏黏度计(见图1)，型号为1B。也可使用在ISO 3105中列出的其他类型黏度计，需保证其测定结果与上述规定的乌氏黏度计相等。有争议时，应使用乌氏黏度计。 5.1.1.2.3 具塞三角烧瓶：100mL。 5.1.1.2.4 移液管或加液器：25mL。 5.1.1.2.5 天平：最小分度值0.1mg。 5.1.1.2.6 过滤器具：不锈钢丝网70μm～120μm或相应的砂芯漏斗。 5.1.1.2.7 计时器：精度0.01s。 5.1.1.2.8 加热装置：温度控制精度2℃。 5.1.1.2.9 真空干燥箱：压力小于133.3Pa，温度控制(105±5)℃。 5.1.1.3 溶剂 5.1.1.3.1 苯酚／1，1，2，2-四氯乙烷(质量比50：50) 两种溶剂以质量比50：50充分混匀，称量精确至少为1％.在(25±0.02)℃时其密度范围为(1.280±0.003)g／cm3。 5.1.1.3.2 苯酚／1，1，2，2-四氯乙烷(质量比60：40) 两种溶剂以质量比60：40充分混匀，称量精确至少为1％。在(25±0.02)℃时其密度范围为(1.235±0.003)g／cm3。 5.1.1.3.3 溶剂的储存 溶剂应保存在棕色玻璃瓶中，避光保存，并保持在(25±2)℃环境温度，避免结晶。严格控制配制好的溶剂含水率小于0.5％。含水率的测试推荐采用GB／T 6283。 注：对于高黏度、高结晶度切片，溶剂的含水率需要加严控制。 5.1.1.3.4 溶剂的选择 PET切片的特性黏度计算方法与所用的溶剂有关。可选用5.1.1.3.1、5.1.1.3.2两种不同的溶剂。 5.1.1.3.5 溶剂稳定性试验 定期重复测量所用溶剂的流出时间。如果溶剂的流出时间超过初始值的1％(初始值为溶剂配制后测量的溶剂流出时间)，则应将溶剂废弃并配制新的溶剂。