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This standard is modified in relation to ASTM D 1321-04 Standard test method for needle penetration of petroleum waxes (English version).
This standard is redrafted in relation to ASTM D 1321-04 Standard test method for needle penetration of petroleum waxes.
Considering China's national conditions, some modifications have been made in this standard with respect to ASTM D 1321-04. The following changes have been made with respect to ASTM D 1321-04:
——The corresponding national standard and professional standard of China are adopted in the normative references of in this standard;
——The Clause 5 "Significance and use" of ASTM D 1319-04 is deleted in this standard;
——The Clause "Keywords" of ASTM D 1319-04 is deleted.
This standard replaces GB/T 4985-1998 Determination of needle penetration of petroleum waxes, and GB/T 4985-1998 is identical to ASTM D 1321-95 Standard test method for needle penetration of petroleum waxes.
The following main changes have been made with respect to GB/T 4985-1998:
——Determination of melting point is added in the Clause "Normative references" in this standard;
——Some contents are added in the Clause "Terms and definitions" in this standard;
——The allowable tolerance of some values is added in this standard;
——This standard cancels The stipulation that "the needle tip just touches the wax surface of the sample for 5min and then releases the plunger";
——Annex A "Small water bath thermostat" and related contents are deleted in this standard;
——The specific technical requirements for water bath thermometers are no longer listed in this standard.
This standard was proposed by the National Technical Committee on Petroleum Products and Lubricants of Standardization Administration of China.
This standard is under the jurisdiction of Subcommittee on Petroleum Wax Products of National Technical Committee on Petroleum Products and Lubricants of Standardization Administration of China.
This standard was issued in March 1985 as first edition, and then revised in June 1998 for the first time and this is the second revision.
Standard test method for needle penetration of petroleum waxes
1 Scope
This standard specifies the empirical estimation of the hardness of waxes derived from petroleum by measurement of the extent of penetration of a standard needle.
This standard is applicable to petroleum waxes having a penetration of not greater than 250.
Note: This test method is similar to the standard test method for penetration of bitumen given in GB/T 4509. See GB/T 269 for determination of cone penetration for lubricating grease and petrolatum.
The values stated in SI units are to be regarded as the standard.
This standard involves some dangerous materials, operations and equipment, but it does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated reference, subsequent amendments to (excluding any corrigendum), or revisions of, any of these publications do not apply. However, parties to agreements based on this standard are encouraged to investigate the possibility of applying the latest editions of the standards indicated below. For undated references, the latest edition of the document referred to applies.
GB/T 514 Specification for liquid-in-glass thermometers for
testing of petroleum products
GB/T 2539 Petroleum waxes-Determination of melting point-Cooling curve method (GB/T 2539-2008, ISO 3841:1977, IDT)
SH/T 0132 Petroleum waxes - Determination of solidification point
3 Terms and definitions
For the purposes of this standard, the following terms and definitions apply.
3.1
penetration of petroleum wax
depth in tenths of a millimetre to which a standard needle penetrates into the wax under defined conditions. As an example, a penetration reading of 85 from the indicator scale corresponds to a penetration depth of 8.5mm
3.2
penetrometer
an instrument that measures the consistency or hardness of semiliquid to semisolid materials by measuring the depth to which a specified cone or needle under a given force falls into the material. In this standard, a standard penetrometer needle (5.3) is used to determine the hardness of petroleum wax. The penetration force is determined by the total mass (100g) of the needle, plunger, and 50g weight
4 Method summary
The sample is heated to at least 17℃ above its expected congealing point or melting point, poured into a container, and then air cooled under controlled conditions. The sample then is conditioned at test temperature in a water bath. Penetration is measured with a penetrometer, which applies a standard needle to the sample for 5s under a load of 100g.
5 Apparatus
5.1 Penetrometer, for applying the standard needle to the surface of the sample specimen and for measuring the extent of penetration at the conclusion of the test. The penetrometer shall be constructed in such a manner that the accurate placement of the tip of the needle at the level surface of the specimen may be made while maintaining a “zero” reading on the indicator. The apparatus shown in Figure 1 represents a composite drawing illustrating the two available types of instrument, one with an adjustable table and the other with an adjustable needle assembly; the use of either type of instrument is permissible. The loaded needle must fall, when released, without appreciable friction. The apparatus shall be provided with leveling screws and a spirit level to maintain the plunger shaft in a true vertical position. The indicator scale shall be calibrated in tenths of a millimetre division and shall have a range of at least 250 tenths of millimetres.
5.2 Timing device
An automatic timing release mechanism attached to the penetrometer may be used. Alternatively, a stop watch graduated in 0.1-s intervals may be used.
5.3 Needle and plunger
The needle shall be approximately 83mm in length and conform to the dimensions shown in Figure 2. It shall be symmetrically tapered at one end to a cone whose angle shall be within the range from 8°55′ to 9°25′ over the entire length of the cone. The axis of the cone shall be coincident with the shaft axis within 0.13-mm maximum runout (total indicator reading). The tapered section of the needle shall be made from fully hardened and tempered stainless steel, Grade 440-C or equal, Rockwell hardness C57 to C60. After tapering, the point shall be ground off to a truncated cone, the smaller base of which shall be from 0.14mm to 0.16mm in diameter. The truncation shall be square with the needle axis within 2°, and the edge shall be sharp and free from burrs. The conical surface and the truncation shall be finished to a smoothness of 0.2µm (rms). The final weight of the needle shall be 2.5g±0.05g (to achieve the required quality by drilling and adjusting the length). The total weight of the plunger shall be 47.5g±0.05g; a weight of 50g±0.05g is required for mounting on the plunger.
Foreword I 1 Scope 2 Normative references 3 Terms and definitions 4 Method summary 5 Apparatus 6 Preparation of test specimen 7 Test procedures 8 Report 9 Precision and bias
ICS 75.140 E 42 中华人民共和国国家标准 GB/T 4985—2010 代替GB/T 4985—1998 石油蜡针入度测定法 Standard test method for needle penetration of petroleum waxes 2010-09-02发布 2010-12-01实施 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 前言 本标准修改采用美国试验与材料协会标准ASTM D1321-04《石油蜡针入度测定法》(英文版)。 本标准根据ASTM D 1321-04《石油蜡针入度测定法》重新起草。 考虑到我国国情，在采用ASTM D 1321-04时，本标准做了一些修改。本标准与ASTM D 1321-04的主要差异： ——本标准规范性引用文件采用了我国相应的国家标准和行业标准； ——本标准删除了ASTM D 1319-04的第5章“意义和用途”； ——本标准取消了ASTM D 1319-04的“关键词”章。 本标准代替GB/T 4985—1998《石油蜡针入度测定法》，GB/T 4985—1998 是等同采用ASTM D 1321-95《石油蜡针入度测定法》制定。 本标准与GB/T 4985—1998的主要差异： ——本标准在“规范性引用文件”章中增加熔点测定法； ——本标准在“术语和定义”章中增加部分内容； ——本标准增加了部分数值的允许公差； ——本标准取消了“针尖恰好接触试样的蜡表面5min后释放滑杆”的规定； ——本标准删除了附录A“小水浴恒温仪”及相关内容； ——本标准不再列出水浴温度计的具体技术要求。 本标准由全国石油产品和润滑剂标准化技术委员会提出。 本标准由全国石油产品和润滑剂标准化技术委员会石油蜡类产品分技术委员会归口。 本标准于1985年3月首次发布，于1998年6月第一次修订，本次为第二次修订。 石油蜡针入度测定法 1 范围 本标准规定了通过测量标准针刺入深度，评价石油蜡硬度的方法。 本标准适用于针入度值不大于250的石油蜡。 注：本方法与测定沥青针入度的GB/T 4509方法相似，润滑脂和石油脂的锥入度测定法见GB/T 269。 本标准采用国际单位制单位。 本标准涉及某些有危险的材料、操作和设备，但是无意对与此有关的所有安全问题都提出建议。因此，使用者在使用本标准之前应建立适当的安全和防护措施，并确定有适用性的管理制度。 2 规范性引用文件 下列文件中的条款通过本标准的引用而成为本标准的条款。凡是注日期的引用文件，其随后所有的修改单(不包括勘误的内容)或修订版均不适用于本标准，然而，鼓励根据本标准达成协议的各方研究是否可使用这些文件的最新版本。凡是不注日期的引用文件，其最新版本适用于本标准。 GB/T 514 石油产品试验用玻璃液体温度计技术条件 GB/T 2539 石油蜡熔点的测定 冷却曲线法(GB/T 2539—2008，ISO 3841：1977，IDT) SH/T 0132 石油蜡冻凝点测定法 3 术语和定义 本标准采用下列术语和定义。 3.1 石油蜡针入度 penetration of petroleum wax 在规定的条件下，标准针垂直刺入蜡试样的深度，以 mm 为单位。例如，针入度计刻度盘示数85表示刺入深度是8.5mm。 3.2 针入度计 penetrometer 用于测定固体或半固体原料稠度或硬度的仪器，测定规定重量的针或锥在重力作用下刺入原料的深度。本标准中，用标准针(5.3)来测定蜡的硬度，总负荷包括标准针、滑杆和50g砝码共100g。 4 方法概要 加热试样至其预期冻凝点或熔点以上至少17℃，倒入成型器中，在控制条件下置于空气中冷却，然后在水浴中将试样温度控制在试验温度，用针入度计测量其针入度，将针入度计的标准针在100g负荷下刺入试样5s。 5 仪器 5.1 针入度计：用于使标准针接触试样表面并且在当试验完结时测量刺入深度。针入度计应按如下方式构建：在指示器读数为“零”时，针尖应能准确置于试样的水平面上。图1中的装置是两种调节方式的组合图：一种带有可调节测试台；另一种带有可调节针组件，二者任选其一。在释放带负荷的针时，针应在无明显的阻力下脱落。仪器上备有水平调节螺丝和水准仪，以保证滑杆轴处于真正的垂直位置。指示器的刻度应标定为 mm，刻度范围应不少于250个 mm。 5.2 计时器 可以使用针入度计附带的自动计时释放机械装置，或者选择精度0.1s的停止秒表。 5.3 标准针和滑杆 标准针的尺寸要求见图2，针长约83mm。针的一末端被对称地逐渐尖细成圆锥形，整个锥体长度的锥角应在8°55′~9°25′范围内，锥体轴与针杆轴重合，最大偏心率(指示器全程刻度)在0.13mm 之内。锥体部分要用充分硬化并回火的不锈钢制作，440-C级或者相当，洛氏硬度C57~C60。锥体渐变细后，磨掉尖端使之成为截顶圆锥体，小头的截面直径为0.14mm~0.16mm。截面与针轴成直角，允许偏离在2°以内，边缘应锐利而无芒刺，锥面与截面顶的光洁度为0.2μm(rms)。标准针的实际质量为2.5g±0.05g(通过杆钻孔和调整长度达到规定质量)，滑杆的总质量为47.5g±0.05g，滑杆上加50g±0.05g的砝码。 注：标准针要经计量部门按上述要求检定。
