[go: up one dir, main page]

CN118777459A - A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times - Google Patents

A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times Download PDF

Info

Publication number
CN118777459A
CN118777459A CN202410929748.3A CN202410929748A CN118777459A CN 118777459 A CN118777459 A CN 118777459A CN 202410929748 A CN202410929748 A CN 202410929748A CN 118777459 A CN118777459 A CN 118777459A
Authority
CN
China
Prior art keywords
insulation
sample
cross
xlpe
linked
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202410929748.3A
Other languages
Chinese (zh)
Inventor
陈悦庆
曾挺
袁明蓬
方戈
王野
倪楚腾
冯洁
吴哲
李华纲
魏腾
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shantou Power Supply Bureau of Guangdong Power Grid Co Ltd
Original Assignee
Shantou Power Supply Bureau of Guangdong Power Grid Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shantou Power Supply Bureau of Guangdong Power Grid Co Ltd filed Critical Shantou Power Supply Bureau of Guangdong Power Grid Co Ltd
Priority to CN202410929748.3A priority Critical patent/CN118777459A/en
Publication of CN118777459A publication Critical patent/CN118777459A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8675Evaluation, i.e. decoding of the signal into analytical information
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N2030/042Standards
    • G01N2030/047Standards external

Landscapes

  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Library & Information Science (AREA)
  • Engineering & Computer Science (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a method for testing the content of cross-linked byproducts in the insulation of a high-voltage XLPE cable under different air-removal temperature and time conditions. The test method comprises the following steps: s1, reserving three parts of conductor shielding, XLPE insulation and insulation shielding for a cable sample; s2, performing heat treatment on the cable sample; s3, cutting a cable integral sample and XLPE insulating inner layer, middle layer and outer layer samples; s4, carrying out heat treatment on the sample; s5, preparing standard solutions with different concentrations by using cumyl alcohol, acetophenone and alpha-methylstyrene, and performing analysis and test by using a gas chromatography-mass spectrometry method to obtain the linear relation between the peak areas and the mass of the three crosslinking byproducts; s6, analyzing and testing the heat-treated sample, and bringing the peak areas of the three crosslinking byproducts into a linear relationship to obtain the concentration of the three crosslinking byproducts in the insulating sample. The invention reflects the air removal effect of the high-voltage XLPE cable by detecting the contents of three crosslinking byproducts in the air-removed sample.

Description

一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交 联副产物含量的测试方法A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times

技术领域:Technical field:

本发明涉及高压XLPE电缆祛气生产工艺技术领域,具体涉及一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法。The invention relates to the technical field of high-voltage XLPE cable degassing production process, and in particular to a method for testing the content of cross-linked byproducts inside the insulation of a high-voltage XLPE cable under different degassing temperature and time conditions.

背景技术:Background technology:

对于高压XLPE电缆,在生产过程中绝缘材料会发生交联反应,绝缘材料由线型结构的热塑性材料转变成网状结构热固性材料,使电缆的运行温度得到了提高。对于高压电缆,主要采用过氧化物交联的方式,最常用的交联剂是过氧化二异丙苯(DCP)。在交联反应的过程中,主要的副产物有枯基醇、苯乙酮、α-甲基苯乙烯、甲烷。这些交联副产物主要以小分子的形式存在于XLPE的无定形区内,造成绝缘缺陷影响电缆的安全运行。因此,需要对高压交联聚乙烯绝缘电缆进行祛气。目前电缆生产厂家主要的祛气方法是将电缆绝缘线芯放在65℃~70℃的专用祛气室中来消除交联反应产生的副产物。For high-voltage XLPE cables, the insulating material undergoes a cross-linking reaction during the production process, and the insulating material is transformed from a linear thermoplastic material to a mesh thermosetting material, which increases the operating temperature of the cable. For high-voltage cables, peroxide cross-linking is mainly used, and the most commonly used cross-linking agent is diisopropylbenzene peroxide (DCP). During the cross-linking reaction, the main by-products are cumyl alcohol, acetophenone, α-methylstyrene, and methane. These cross-linking by-products mainly exist in the amorphous region of XLPE in the form of small molecules, causing insulation defects that affect the safe operation of the cable. Therefore, it is necessary to degas the high-voltage cross-linked polyethylene insulated cable. At present, the main degassing method of cable manufacturers is to place the cable insulation core in a special degassing chamber at 65℃~70℃ to eliminate the by-products produced by the cross-linking reaction.

不同电压等级的电缆的绝缘厚度各不同,因此电缆的祛气时间也各不相同。但目前的电缆祛气时间大都根据经验确定,缺少电缆祛气程度的评价指标,因此需要一种有效的检测高压XLPE电缆绝缘内部交联副产物含量的方法,对XLPE内部交联副产物的浓度进行准确的定量,从而在此基础上建立祛气程度的评价指标。现有的高压XLPE电缆祛气效果的检测方法主要包括检测绝缘线芯内部空间电荷特性和检测交联副产物的残留量,其方法包括称重法和采用热失重分析仪对交联副产物进行检测,还有利用气相色谱仪检测祛气室中气体成分及含量。这些方法虽然能够测定交联副产物的大致残留量,但是不能准确定量。而气相色谱-质谱(GC-MS)仪器可以提供质谱可用于识别身份已知或者未知的化合物,还提供可用于定性和定量分析的色谱图,可以得到交联副产物的具体残留量,有利于评价高压电缆祛气效果。所以,有必要提出一种基于相色谱-质谱联用法的高效准确的不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法。The insulation thickness of cables of different voltage levels is different, so the degassing time of the cables is also different. However, the current cable degassing time is mostly determined based on experience, and there is a lack of evaluation indicators for the degree of cable degassing. Therefore, an effective method for detecting the content of cross-linked by-products in the insulation of high-voltage XLPE cables is needed to accurately quantify the concentration of cross-linked by-products inside XLPE, so as to establish an evaluation index for the degree of degassing on this basis. The existing methods for detecting the degassing effect of high-voltage XLPE cables mainly include detecting the internal space charge characteristics of the insulation core and detecting the residual amount of cross-linked by-products. The methods include weighing and using a thermogravimetric analyzer to detect the cross-linked by-products, and using a gas chromatograph to detect the gas composition and content in the degassing chamber. Although these methods can determine the approximate residual amount of cross-linked by-products, they cannot be accurately quantified. The gas chromatography-mass spectrometry (GC-MS) instrument can provide a mass spectrum that can be used to identify compounds with known or unknown identities, and also provides a chromatogram that can be used for qualitative and quantitative analysis. The specific residual amount of cross-linked by-products can be obtained, which is conducive to evaluating the degassing effect of high-voltage cables. Therefore, it is necessary to propose an efficient and accurate test method for the content of internal cross-linking by-products in high-voltage XLPE cable insulation under different degassing temperatures and time conditions based on liquid chromatography-mass spectrometry.

发明内容:Summary of the invention:

本发明解决了现有技术存在的问题,提供一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法,本发明提出的测试方法可以准确检测出XLPE绝缘内部枯基醇、苯乙酮和α-甲基苯乙烯三种交联副产物的浓度,从而建立高压电缆祛气效果的评价指标,可以更有效地指导高压XLPE电缆的生产。The present invention solves the problems existing in the prior art and provides a method for testing the content of cross-linked by-products in the insulation of a high-voltage XLPE cable under different degassing temperature and time conditions. The testing method proposed by the present invention can accurately detect the concentrations of three cross-linked by-products, namely, cumyl alcohol, acetophenone and alpha-methylstyrene, in the XLPE insulation, thereby establishing an evaluation index for the degassing effect of the high-voltage cable, and can more effectively guide the production of the high-voltage XLPE cable.

本发明的目的是提供一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法,包括如下步骤:The object of the present invention is to provide a method for testing the content of cross-linked byproducts in the insulation of a high-voltage XLPE cable under different degassing temperatures and time conditions, comprising the following steps:

S1、将电缆试样去除导体和半导电尼龙带、半导电多特带部分,保留导体屏蔽、XLPE绝缘和绝缘屏蔽三个部分;S1. Remove the conductor, semi-conductive nylon tape and semi-conductive multi-tape parts from the cable sample, and keep the conductor shield, XLPE insulation and insulation shield;

S2、将电缆试样分为两组,分别对电缆试样进行热处理;S2. Divide the cable samples into two groups and perform heat treatment on the cable samples respectively;

S3、将热处理后的电缆试样进一步切割,分别切取包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品以及XLPE绝缘的内层、中层和外层样品;S3, further cutting the heat-treated cable sample to obtain the whole cable sample including the conductor shield, XLPE insulation, insulation shield, and the inner layer, middle layer and outer layer samples of the XLPE insulation;

S4、将电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品进行热处理;S4, heat treating the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation;

S5、利用枯基醇、苯乙酮和α-甲基苯乙烯三种分析测试标准品,配置不同浓度的标准溶液,利用气相色谱-质谱联用法,对不同浓度的标准溶液进行分析测试,得到标准溶液中枯基醇、苯乙酮、α-甲基苯乙烯三种交联副产物的峰面积与质量的线性关系;S5. Using three analytical test standards, namely, cumyl alcohol, acetophenone and α-methylstyrene, standard solutions of different concentrations are prepared, and the standard solutions of different concentrations are analyzed and tested by gas chromatography-mass spectrometry to obtain a linear relationship between the peak area and mass of the three cross-linking byproducts of cumyl alcohol, acetophenone and α-methylstyrene in the standard solution;

S6、利用气相色谱-质谱联用法,对步骤S4热处理后的电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品分别进行分析测试,将样品测试中测得的三种交联副产物的峰面积带入此线性关系,得到三种交联副产物在绝缘样品中的浓度。S6. Using gas chromatography-mass spectrometry, the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation after the heat treatment in step S4 are analyzed and tested respectively, and the peak areas of the three cross-linked by-products measured in the sample test are brought into this linear relationship to obtain the concentrations of the three cross-linked by-products in the insulation sample.

本发明通过热处理模拟电缆祛气过程,得到样品中交联副产物随加热时间的变化规律。本发明通过检测祛气后样品中枯基醇、苯乙酮和α-甲基苯乙烯三种交联副产物的含量来反映高压XLPE电缆的祛气效果。The present invention simulates the cable degassing process by heat treatment to obtain the variation law of crosslinked byproducts in the sample with heating time. The present invention reflects the degassing effect of the high-voltage XLPE cable by detecting the contents of three crosslinked byproducts, namely cumyl alcohol, acetophenone and α-methylstyrene, in the degassing sample.

优选地,步骤S2具体包括如下步骤:Preferably, step S2 specifically includes the following steps:

S21、将样品分成两组,每组若干段样品,分别标号A、B;S21, divide the samples into two groups, each group has several sections of samples, labeled A and B respectively;

S22、A、B两组各保留一个样品,将其他样品置于恒温箱进行模拟祛气,两组A、B热处理的温度分别设定65℃和70℃,每间隔12h取样一次,祛气周期为144h。One sample was retained from each of the two groups S22, A, and B, and the other samples were placed in a constant temperature box for simulated degassing. The heat treatment temperatures of the two groups A and B were set at 65°C and 70°C, respectively. Sampling was taken every 12 hours, and the degassing cycle was 144 hours.

优选地,步骤S3的具体步骤为:用电缆切割机切取扇形的包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品,得到电缆整体样品;制取XLPE绝缘的内层、中层和外层样品时,在电缆整体样品的基础上,去除导体屏蔽、绝缘屏蔽,剩下XLPE绝缘部分,然后平行于弧面切成三等份,由内向外分别为XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品。Preferably, the specific steps of step S3 are: using a cable cutter to cut a fan-shaped whole cable sample including a conductor shield, XLPE insulation, and an insulation shield to obtain a whole cable sample; when preparing the inner, middle, and outer layer samples of the XLPE insulation, on the basis of the whole cable sample, remove the conductor shield and the insulation shield, leaving the XLPE insulation part, and then cut it into three equal parts parallel to the arc surface, which are the inner layer of the XLPE insulation, the middle layer of the XLPE insulation, and the outer layer of the XLPE insulation from the inside to the outside.

优选地,步骤S4的具体步骤为:将电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品分装在顶空瓶中,利用恒温热烘箱进行热处理,热处理的条件是:加热温度120℃,加热时间5h。Preferably, the specific steps of step S4 are: packing the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation in headspace bottles, and heat treating them in a constant temperature oven, and the heat treatment conditions are: heating temperature 120° C., heating time 5 h.

优选地,步骤S5中:将枯基醇分别配置成0.2mg/mL、0.4mg/mL、1.0mg/mL、2.0mg/mL、4.0mg/mL、20.0mg/mL 6种不同浓度的标准溶液,苯乙酮分别配置成0.3mg/mL、0.6mg/mL、1.5mg/mL、3.0mg/mL、6.0mg/mL、30.0mg/mL 6种不同浓度的标准溶液,α-甲基苯乙烯分别配置成0.02mg/mL、0.04mg/mL、0.1mg/mL、0.2mg/mL、0.4mg/mL、2.0mg/mL 6种不同浓度的标准溶液。Preferably, in step S5: cumyl alcohol is respectively configured into 6 standard solutions of different concentrations of 0.2 mg/mL, 0.4 mg/mL, 1.0 mg/mL, 2.0 mg/mL, 4.0 mg/mL, and 20.0 mg/mL; acetophenone is respectively configured into 6 standard solutions of different concentrations of 0.3 mg/mL, 0.6 mg/mL, 1.5 mg/mL, 3.0 mg/mL, 6.0 mg/mL, and 30.0 mg/mL; α-methylstyrene is respectively configured into 6 standard solutions of different concentrations of 0.02 mg/mL, 0.04 mg/mL, 0.1 mg/mL, 0.2 mg/mL, 0.4 mg/mL, and 2.0 mg/mL.

优选地,步骤S5具体包括如下步骤:Preferably, step S5 specifically includes the following steps:

S51、用气相色谱质谱联用仪检测样品与6种不同浓度的标准溶液,得到每一种交联副产物在6种不同浓度下的峰面积,将6个测试数据与原点记录在坐标平面上,拟合出每一种交联副产物对应的回归方程y=kx+b,其中纵坐标y代表交联副产物质量,横坐标x代表交联副产物峰面积,回归方程参数求解公式如下:S51. Use gas chromatography-mass spectrometry to detect the sample and 6 standard solutions of different concentrations, obtain the peak area of each cross-linked by-product at 6 different concentrations, record the 6 test data and the origin on the coordinate plane, and fit the regression equation y=kx+b corresponding to each cross-linked by-product, where the ordinate y represents the mass of the cross-linked by-product, and the abscissa x represents the peak area of the cross-linked by-product. The regression equation parameter solution formula is as follows:

优选地,步骤S6具体包括如下步骤:Preferably, step S6 specifically includes the following steps:

S61、采用外标法,根据交联副产物峰面积与质量的关系曲线,计算样品中各种交联副产物的浓度,公式如下:S61. Using the external standard method, the concentration of various cross-linking by-products in the sample is calculated based on the relationship curve between the peak area and mass of the cross-linking by-products. The formula is as follows:

其中,ci表示交联副产物i的浓度,i包括α-甲基苯乙烯、苯乙酮和枯基醇,单位为mg/g;ki表示交联副产物i标准曲线的斜率,单位为mg;mj表示第j个样品的质量,单位为g;Aji表示第j个样品中交联副产物i的峰面积,无单位。Wherein, ci represents the concentration of cross-linked by-product i, i includes α-methylstyrene, acetophenone and cumyl alcohol, and the unit is mg/g; ki represents the slope of the standard curve of cross-linked by-product i, and the unit is mg; mj represents the mass of the j-th sample, and the unit is g; Aji represents the peak area of cross-linked by-product i in the j-th sample, and the unit is unitless.

优选地,步骤S5或S6所述的气相色谱-串联质谱法检测条件:色谱柱为HP-INNOWax,规格为30m×0.25mm×0.25μm;进样口温度为250℃;Preferably, the gas chromatography-tandem mass spectrometry detection conditions described in step S5 or S6 are: the chromatographic column is HP-INNOWax, with specifications of 30m×0.25mm×0.25μm; the injection port temperature is 250°C;

升温程序:初始温度40℃,保持3min,以10℃/min升温至250℃,保持5min;Heating program: initial temperature 40°C, hold for 3 min, increase to 250°C at 10°C/min, hold for 5 min;

所用载气为纯度为99.9995%的氦气,氦气流速为1mL/min;进样方式为分流进样,分流比30:1,进样量为100μL;质谱采集方式为scan模式,m/z范围是33-500。The carrier gas used was helium with a purity of 99.9995% and a helium flow rate of 1 mL/min; the injection method was split injection with a split ratio of 30:1 and an injection volume of 100 μL; the mass spectrometry acquisition method was scan mode with an m/z range of 33-500.

本发明还保护所述的测试方法在测试不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量中的应用。The present invention also protects the application of the test method in testing the content of cross-linked byproducts inside the insulation of a high-voltage XLPE cable under different degassing temperature and time conditions.

本发明与现有技术相比,具有如下优点:本发明利用气相色谱质谱联用仪对XLPE样品的交联副产物成分及含量进行检测和分析,能够准确定量,得到α-甲基苯乙烯、苯乙酮、枯基醇三种交联副产物在XLPE绝缘中的浓度,使评估更准确高效;本发明分析不同祛气温度和祛气时间下交联副产物的含量,得到交联副产物在祛气过程中含量变化的规律。Compared with the prior art, the present invention has the following advantages: the present invention uses a gas chromatography-mass spectrometer to detect and analyze the cross-linked by-product components and contents of XLPE samples, and can accurately quantify and obtain the concentrations of three cross-linked by-products, namely, alpha-methylstyrene, acetophenone, and cumyl alcohol, in XLPE insulation, so that the evaluation is more accurate and efficient; the present invention analyzes the contents of cross-linked by-products at different degassing temperatures and degassing times, and obtains the law of content changes of cross-linked by-products during the degassing process.

附图说明:Description of the drawings:

图1是本发明提出的测试方法的流程图;FIG1 is a flow chart of the testing method proposed by the present invention;

图2是样品的取样方法及规格;Figure 2 shows the sampling method and specifications of the samples;

图3是顶空瓶测试样品制样方法;Fig. 3 is a headspace bottle test sample preparation method;

图4是气相色谱质谱联用仪原理图;Fig. 4 is a schematic diagram of a gas chromatography-mass spectrometer;

图5是配置标准溶液示意图;Fig. 5 is a schematic diagram of configuring a standard solution;

图6是实施例1中标准溶液峰面积-质量关系;Fig. 6 is the peak area-mass relationship of the standard solution in Example 1;

图7是不同祛气时间的样品测试结果;FIG7 is a test result of samples with different degassing times;

附图标记说明:1、导体;2、半导体尼龙带+半导体特多龙带层;3、导体屏蔽层;4、XLPE绝缘层;41、绝缘内层;42、绝缘中层;43、绝缘外层;5、绝缘屏蔽层。Explanation of the reference numerals: 1. conductor; 2. semiconductor nylon tape + semiconductor terylene tape layer; 3. conductor shielding layer; 4. XLPE insulation layer; 41. insulation inner layer; 42. insulation middle layer; 43. insulation outer layer; 5. insulation shielding layer.

具体实施方式:Specific implementation method:

以下实施例是对本发明的进一步说明,而不是对本发明的限制。The following examples are provided to further illustrate the present invention, rather than to limit the present invention.

除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。除特别说明,本文中的实验材料和试剂均为本技术领域常规市购产品。Unless otherwise defined, all professional terms used hereinafter have the same meaning as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention. Unless otherwise specified, the experimental materials and reagents herein are conventional commercial products in the art.

如图1-5所示,电缆试样由内到外依次包括导体1、半导体尼龙带+半导体特多龙带层2;导体屏蔽层3、XLPE绝缘层4和绝缘屏蔽层5,XLPE绝缘层4从内到外依次为绝缘内层41、绝缘中层42和绝缘外层43。As shown in FIGS. 1-5 , the cable sample includes, from the inside to the outside, a conductor 1, a semiconductor nylon tape + a semiconductor terylene tape layer 2; a conductor shielding layer 3, an XLPE insulation layer 4 and an insulation shielding layer 5. The XLPE insulation layer 4 includes, from the inside to the outside, an insulation inner layer 41, an insulation middle layer 42 and an insulation outer layer 43.

一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法,通过检测祛气后样品中枯基醇、苯乙酮和α-甲基苯乙烯三种交联副产物的含量来反映高压XLPE电缆的祛气效果,上述测试方法包括以下步骤:A method for testing the content of cross-linked byproducts in the insulation of a high-voltage XLPE cable under different degassing temperatures and time conditions, which reflects the degassing effect of the high-voltage XLPE cable by detecting the contents of three cross-linked byproducts, namely, cumyl alcohol, acetophenone and α-methylstyrene, in the degassing sample. The testing method comprises the following steps:

S1、利用电缆切割机切取长20mm的电缆试样,去除导体和半导电尼龙带、半导电多特带部分,保留导体屏蔽、XLPE绝缘和绝缘屏蔽三个部分;S1. Use a cable cutter to cut a 20 mm long cable sample, remove the conductor and semi-conductive nylon tape, and semi-conductive multi-tape, and keep the conductor shield, XLPE insulation, and insulation shield.

S2、将电缆试样分为两组,利用恒温热烘箱对电缆绝缘试样进行加热处理,设置加热温度为65℃和70℃,每间隔12h取样一次,祛气周期为144h;S2. Divide the cable samples into two groups, and heat the cable insulation samples in a constant temperature oven. Set the heating temperature to 65℃ and 70℃, take samples every 12h, and the degassing cycle is 144h;

S3、将恒温烘箱中取出的绝缘样品进一步切割,分别切取包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品以及XLPE绝缘的内层、中层和外层样品,称量样品质量;S3, further cutting the insulation samples taken out of the constant temperature oven, cutting out the whole cable samples including the conductor shield, XLPE insulation, insulation shield, and the inner layer, middle layer and outer layer samples of the XLPE insulation, and weighing the sample masses;

S4、将不同的绝缘样品分装在20mL顶空瓶中,利用恒温热烘箱进行热处理,加热温度120℃,加热时间5h;S4. Different insulation samples were packed into 20 mL headspace bottles and heat treated in a constant temperature oven at 120 °C for 5 h.

S5、利用浓度大于99%的枯基醇、苯乙酮和α-甲基苯乙烯三种分析测试标准品,配置6种不同浓度的标准溶液,分别取50μL分装于20mL顶空瓶中;利用气相色谱-质谱联用法,对不同浓度的标准溶液进行分析测试,得到标准溶液中枯基醇、苯乙酮、α-甲基苯乙烯三种交联副产物的峰面积与质量的线性关系;S5. Using three analytical test standards of cumyl alcohol, acetophenone and α-methylstyrene with a concentration greater than 99%, 6 standard solutions of different concentrations were prepared, and 50 μL of each solution was dispensed into a 20 mL headspace bottle; using gas chromatography-mass spectrometry, the standard solutions of different concentrations were analyzed and tested to obtain the linear relationship between the peak area and mass of the three cross-linking byproducts of cumyl alcohol, acetophenone and α-methylstyrene in the standard solution;

S6、利用气相色谱-质谱联用法,对步骤S4热处理后的电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品分别进行分析测试,将样品测试中测得的三种交联副产物的峰面积带入此线性关系,得到三种交联副产物在绝缘样品中的浓度。S6. Using gas chromatography-mass spectrometry, the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation after the heat treatment in step S4 are analyzed and tested respectively, and the peak areas of the three cross-linked by-products measured in the sample test are brought into this linear relationship to obtain the concentrations of the three cross-linked by-products in the insulation sample.

步骤S1的具体步骤为:The specific steps of step S1 are:

S11、用电缆切割机切取20mm的XLPE样品之后,将样品水平固定,用锤子对位于内部的导体多次敲击,直致导体脱落。然后撕去位于内表面的半导电尼龙带、半导电特多龙带部分。使样品只包含导体屏蔽、XLPE绝缘和绝缘屏蔽三层结构,一共制得26段样品。S11. Cut a 20 mm XLPE sample with a cable cutter, fix the sample horizontally, and use a hammer to hit the conductor inside for several times until the conductor falls off. Then tear off the semi-conductive nylon tape and semi-conductive terylene tape on the inner surface. Make the sample only contain the three-layer structure of conductor shielding, XLPE insulation and insulation shielding, and prepare 26 samples in total.

步骤S2的具体步骤为:The specific steps of step S2 are:

S21、将样品分成两组,每组13段样品,分别标号A、B。S21. Divide the samples into two groups, each with 13 samples, labeled A and B respectively.

S22、A、B两组各保留一个样品,将其他样品置于恒温箱进行模拟祛气。两组分别设定65℃和70℃。One sample was kept in each of the two groups S22, A, and B, and the other samples were placed in a constant temperature box for simulated degassing. The two groups were set at 65℃ and 70℃ respectively.

S23、摆放样品时均匀排列在恒温箱底层,所有样品位于同一水平平面,以保证样品受热均匀。S23. Arrange the samples evenly on the bottom layer of the constant temperature box, with all samples located on the same horizontal plane to ensure that the samples are heated evenly.

步骤S3的具体步骤为:The specific steps of step S3 are:

S31、用电缆切割机切取扇形的包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品,得到电缆整体样品。制取XLPE绝缘的内层、中层和外层样品时,在电缆整体样品的基础上,去除导体屏蔽、绝缘屏蔽,剩下XLPE绝缘部分。然后平行于弧面切成三等份,由内向外分别为XLPE绝缘的内层、XLPE绝缘中层和XLPE绝缘外层样品。S31. Cut a fan-shaped cable sample including conductor shielding, XLPE insulation, and insulation shielding with a cable cutter to obtain a cable sample. When preparing the inner, middle, and outer layer samples of XLPE insulation, remove the conductor shielding and insulation shielding on the basis of the cable sample, leaving the XLPE insulation part. Then cut it into three equal parts parallel to the arc surface, from the inside to the outside, respectively, the inner layer of XLPE insulation, the middle layer of XLPE insulation, and the outer layer of XLPE insulation.

S32、称取样品质量时使用电子天平。先清洁样品表面,然后将电子天平置零,避免系统误差。再将样品置于电子天平上称重,称重时关闭电子天平的玻璃窗口,避免干扰。S32. Use an electronic balance to weigh the sample. Clean the sample surface first, then set the electronic balance to zero to avoid system errors. Then place the sample on the electronic balance and weigh it. Close the glass window of the electronic balance during weighing to avoid interference.

步骤S4的具体步骤为:The specific steps of step S4 are:

S41、加热时所有顶空瓶放置于不锈钢样品瓶架上并整齐排列于烘箱底层,保证受热温度均匀。S41. During heating, all headspace bottles are placed on a stainless steel sample bottle rack and neatly arranged on the bottom layer of the oven to ensure uniform heating temperature.

步骤S5的具体步骤为:The specific steps of step S5 are:

S51、配置标准溶液:先用移液枪对α-甲基苯乙烯、苯乙酮、枯基醇进行取样,移液至5mL的容量瓶1中并称量质量,三种标准物的质量分别是10mg、150mg、100mg。再加入甲醇溶液至容量瓶刻度线处,得到标样1,以此为母液进行稀释。用移液枪取1mL母液至5mL的容量瓶2,加入甲醇溶液稀释至容量瓶刻度线处,得到标样2。用移液枪取1mL母液至10mL的容量瓶3,加入甲醇溶液稀释至容量瓶刻度线处,得到标样3。用移液枪取0.5mL母液至10mL的容量瓶4,加入甲醇溶液稀释至容量瓶刻度线处,得到标样4。用移液枪取1mL标样2至10mL的容量瓶,加入甲醇溶液稀释至容量瓶刻度线处,得到标样5。用移液枪取1mL标样3至10mL的容量瓶,加入甲醇溶液稀释至容量瓶刻度线处,得到标样6。S51. Prepare standard solutions: first use a pipette to sample α-methylstyrene, acetophenone, and cumyl alcohol, pipette them into a 5mL volumetric flask 1, and weigh the masses. The masses of the three standards are 10mg, 150mg, and 100mg, respectively. Then add methanol solution to the scale line of the volumetric flask to obtain standard sample 1, which is used as the mother solution for dilution. Use a pipette to take 1mL of the mother solution to a 5mL volumetric flask 2, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 2. Use a pipette to take 1mL of the mother solution to a 10mL volumetric flask 3, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 3. Use a pipette to take 0.5mL of the mother solution to a 10mL volumetric flask 4, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 4. Use a pipette to take 1mL of standard sample 2 to a 10mL volumetric flask, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 5. Use a pipette to transfer 1 mL of standard sample 3 to a 10 mL volumetric flask, add methanol solution and dilute to the mark on the volumetric flask to obtain standard sample 6.

S52、用气相色谱质谱联用仪检测样品与6种不同浓度的标准液,得到每一种交联副产物在6种不同浓度下的峰面积,将6个测试数据与原点记录在坐标平面上,拟合出每一种交联副产物对应的回归方程y=kx+b,其中纵坐标y代表交联副产物质量,横坐标x代表交联副产物峰面积,回归方程参数求解公式如下:S52. Use gas chromatography-mass spectrometry to detect the sample and 6 standard solutions of different concentrations, obtain the peak area of each cross-linked by-product at 6 different concentrations, record the 6 test data and the origin on the coordinate plane, and fit the regression equation y=kx+b corresponding to each cross-linked by-product, where the ordinate y represents the mass of the cross-linked by-product, and the abscissa x represents the peak area of the cross-linked by-product. The regression equation parameter solution formula is as follows:

步骤S6的具体步骤为:The specific steps of step S6 are:

S61、采用外标法,根据交联副产物峰面积与质量的关系曲线,计算样品中各种交联副产物的浓度。公式如下:S61. Using the external standard method, the concentration of various cross-linking by-products in the sample is calculated based on the relationship curve between the peak area and mass of the cross-linking by-products. The formula is as follows:

其中,ci表示交联副产物i(包括α-甲基苯乙烯、苯乙酮和枯基醇)的浓度,单位为mg/g;ki表示交联副产物i标准曲线的斜率,单位为mg;mj表示第j个样品的质量,单位为g;Aji表示第j个样品中交联副产物i的峰面积,无单位。Wherein, ci represents the concentration of cross-linked by-product i (including α-methylstyrene, acetophenone and cumyl alcohol), in mg/g; ki represents the slope of the standard curve of cross-linked by-product i, in mg; mj represents the mass of the j-th sample, in g; Aji represents the peak area of cross-linked by-product i in the j-th sample, without unit.

实施例1Example 1

一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法,包括以下具体步骤:A method for testing the content of cross-linked byproducts in the insulation of a high-voltage XLPE cable under different degassing temperatures and time conditions comprises the following specific steps:

S1、利用电缆切割机切取长20mm的未经祛气处理的110kV XLPE绝缘电缆试样,电缆规格如表1所示。将电缆试样水平固定,用锤子反复敲击中部导体部分直致导体脱落,再撕去内层的半导电尼龙带、半导电特多龙带部分,使试样只包含导体屏蔽、XLPE绝缘和绝缘屏蔽三层结构。取样方法如图2所示。共取26段样品。S1. Use a cable cutter to cut a 20mm long 110kV XLPE insulated cable sample that has not been degassed. The cable specifications are shown in Table 1. Fix the cable sample horizontally, hit the central conductor part repeatedly with a hammer until the conductor falls off, and then tear off the inner semi-conductive nylon tape and semi-conductive terylene tape, so that the sample only contains the three-layer structure of conductor shield, XLPE insulation and insulation shield. The sampling method is shown in Figure 2. A total of 26 samples were taken.

S2、将样品进行模拟祛气处理。实验室模拟祛气试验中,将26段式样分为A、B两组,每组13段式样。每组各保留一段作为对照,然后将A组剩余的12段样品放置于65℃恒温烘箱中进行加热,而B组剩余的12段样品放置于70℃恒温烘箱中进行加热,模拟祛气过程。摆放样品时,将样品均匀排列在恒温箱底层,12段样品在同一水平平面,保证每段样品受热均匀。每间隔12h分别对各组样品取样一次。两组第一次取样时间均是12h,祛气周期是144h。S2. Subject the samples to simulated degassing treatment. In the laboratory simulated degassing test, the 26 sections of samples were divided into two groups, A and B, with 13 sections in each group. One section was retained in each group as a control, and then the remaining 12 sections of samples in group A were placed in a 65°C constant temperature oven for heating, while the remaining 12 sections of samples in group B were placed in a 70°C constant temperature oven for heating to simulate the degassing process. When placing the samples, arrange the samples evenly on the bottom layer of the constant temperature oven, with the 12 sections of samples on the same horizontal plane to ensure that each section of the sample is heated evenly. Samples were taken from each group of samples once every 12 hours. The first sampling time for both groups was 12 hours, and the degassing cycle was 144 hours.

S3、模拟祛气之后进行再次制样。将预先保留的未祛气样品以及模拟祛气后的A、B两组样品进一步切割。每一段试样分别切取包含导体屏蔽、XLPE绝缘和绝缘屏蔽三层结构的绝缘整体样品以及绝缘内层、绝缘中层和绝缘外层四种样品。具体制样方法:用电缆切割机在每段样品上切取一块扇形的包含导体屏蔽、XLPE绝缘和绝缘屏蔽三层结构的绝缘整体,得到整体样品。制取绝缘内层、绝缘中层和绝缘外层时,以整体绝缘样品为基础,切去导体屏蔽和绝缘屏蔽,只剩下XLPE绝缘部分,然后平行于弧面切成三等份,层间间隔5mm,由内向外分别为XLPE绝缘的内层、中层和外层样品。制样方式如图3所示。制样完成后用电子天平称重。先清洁样品表面,然后将电子天平置零,避免系统误差。再将样品置于电子天平上称重,称重时闭合电子天平玻璃窗口,避免干扰。样品质量控制在1.5~3g。若质量过大,则会导致使用气相色谱质谱仪检测出的峰面积过大,且检测时过多的交联副产物会吸附在仪器内壁上,使下次检测的数据偏大,影响实验的准确性。若质量过小,则会导致检测时峰面积偏小,与杂峰混淆,不好辨别。所以要控制好待测样品的质量,以保证数据的准确性。制好的条状样品记录下质量之后,装入20mL螺纹口顶空瓶中,编上序号,共计104个样品。S3. Prepare the sample again after simulated degassing. The previously reserved undegassed samples and the two groups of samples A and B after simulated degassing are further cut. Each section of the sample is cut into four samples: the whole insulation sample with a three-layer structure of conductor shielding, XLPE insulation and insulation shielding, and the inner insulation layer, middle insulation layer and outer insulation layer. Specific sample preparation method: Use a cable cutter to cut a fan-shaped insulation whole with a three-layer structure of conductor shielding, XLPE insulation and insulation shielding from each section of the sample to obtain a whole sample. When preparing the inner insulation layer, middle insulation layer and outer insulation layer, the conductor shielding and insulation shielding are cut off based on the whole insulation sample, leaving only the XLPE insulation part, and then cut into three equal parts parallel to the arc surface, with a layer interval of 5mm, from the inside to the outside, they are the inner layer, middle layer and outer layer samples of XLPE insulation. The sample preparation method is shown in Figure 3. After the sample preparation is completed, weigh it with an electronic balance. Clean the sample surface first, then set the electronic balance to zero to avoid system errors. Then place the sample on the electronic balance for weighing, and close the glass window of the electronic balance during weighing to avoid interference. The sample mass is controlled at 1.5 to 3 g. If the mass is too large, the peak area detected by the gas chromatograph mass spectrometer will be too large, and too many cross-linked byproducts will be adsorbed on the inner wall of the instrument during detection, making the data of the next detection larger, affecting the accuracy of the experiment. If the mass is too small, the peak area will be small during detection, which will be confused with the miscellaneous peaks and difficult to distinguish. Therefore, the mass of the sample to be tested must be controlled to ensure the accuracy of the data. After recording the mass of the prepared strip sample, it is placed in a 20 mL threaded headspace bottle and numbered, for a total of 104 samples.

S4、检测交联副产物成分及含量。首先用α-甲基苯乙烯、苯乙酮和枯基醇三种物质的分析测试标准品作为溶质,用甲醇溶液作为溶剂,配置6种不同浓度的标准溶液,标准溶液浓度如表2所示。具体配置过程如下:先用移液枪分别对α-甲基苯乙烯、苯乙酮、枯基醇进行取样,移液至5mL的容量瓶1中并称量质量,三种标准物的质量分别是10mg、150mg、100mg。再加入甲醇溶液至容量瓶刻度线处,得到标样1,以此为母液进行稀释。用移液枪取1mL母液至5mL的容量瓶2,加入甲醇溶液稀释至容量瓶刻度线处,得到标样2。用移液枪取1mL母液至10mL的容量瓶3,加入甲醇溶液稀释至容量瓶刻度线处,得到标样3。用移液枪取0.5mL母液至10mL的容量瓶4,加入甲醇溶液稀释至容量瓶刻度线处,得到标样4。用移液枪取1mL标样2至10mL的容量瓶,加入甲醇溶液稀释至容量瓶刻度线处,得到标样5。用移液枪取1mL标样3至10mL的容量瓶,加入甲醇溶液稀释至容量瓶刻度线处,得到标样6。配置流程图如下图4所示,标准浓度溶液如表2所示。从6种标准溶液中分别取50μL,分装在顶空瓶中并编号,以备测试。S4, detect the composition and content of cross-linked by-products. First, use the analytical test standards of three substances, α-methylstyrene, acetophenone and cumyl alcohol, as solutes, and use methanol solution as solvent to prepare 6 standard solutions of different concentrations. The concentrations of the standard solutions are shown in Table 2. The specific configuration process is as follows: First, use a pipette to sample α-methylstyrene, acetophenone, and cumyl alcohol, pipette them into a 5mL volumetric flask 1 and weigh the mass. The masses of the three standards are 10mg, 150mg, and 100mg, respectively. Then add methanol solution to the scale line of the volumetric flask to obtain standard sample 1, which is used as the mother liquor for dilution. Use a pipette to take 1mL of mother liquor to a 5mL volumetric flask 2, add methanol solution and dilute to the scale line of the volumetric flask to obtain standard sample 2. Use a pipette to take 1mL of mother liquor to a 10mL volumetric flask 3, add methanol solution and dilute to the scale line of the volumetric flask to obtain standard sample 3. Use a pipette to take 0.5mL of the mother solution to a 10mL volumetric flask 4, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 4. Use a pipette to take 1mL of standard sample 2 to a 10mL volumetric flask, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 5. Use a pipette to take 1mL of standard sample 3 to a 10mL volumetric flask, add methanol solution to dilute to the scale line of the volumetric flask, and obtain standard sample 6. The configuration flow chart is shown in Figure 4 below, and the standard concentration solutions are shown in Table 2. Take 50μL from each of the 6 standard solutions, dispense them into headspace bottles and number them for testing.

S5、采用Agilent GCMS 7890B-7000C气相色谱质谱联用仪,其使用原理如图5所示,对标准溶液样品和104个试验样品进行分析测试,气相色谱-串联质谱法检测条件:色谱柱为HP-INNOWax,规格为30m×0.25mm×0.25μm;进样口温度为250℃;升温程序:初始温度40℃,保持3min,以10℃/min升温至250℃,保持5min;所用载气为纯度为99.9995%的氦气,氦气流速为1mL/min;进样方式为分流进样,分流比30:1,进样量为100μL;质谱采集方式为scan模式,m/z范围是33-500。得到6个标准溶液中三种交联副产物的质量与峰面积的关系(如图6所示),将6个峰面积与原点记录在坐标图中,拟合出每一种交联副产物对应的回归方程y=kx+b,其中纵坐标y代表交联副产物质量,横坐标x代表交联副产物峰面积,回归方程参数求解公式如下:S5. Agilent GCMS 7890B-7000C gas chromatograph-mass spectrometer, whose operating principle is shown in Figure 5, was used to analyze and test the standard solution sample and 104 test samples. The detection conditions of gas chromatography-tandem mass spectrometry were as follows: the chromatographic column was HP-INNOWax with a specification of 30m×0.25mm×0.25μm; the injection port temperature was 250°C; the heating program was as follows: the initial temperature was 40°C, maintained for 3min, and then heated to 250°C at a rate of 10°C/min and maintained for 5min; the carrier gas used was helium with a purity of 99.9995%, and the helium flow rate was 1mL/min; the injection mode was split injection with a split ratio of 30:1 and an injection volume of 100μL; the mass spectrometry acquisition mode was scan mode, and the m/z range was 33-500. The relationship between the mass and peak area of the three cross-linked by-products in the six standard solutions was obtained (as shown in FIG6 ), and the six peak areas and the origin were recorded in a coordinate graph, and the regression equation y=kx+b corresponding to each cross-linked by-product was fitted, where the ordinate y represents the mass of the cross-linked by-product, and the abscissa x represents the peak area of the cross-linked by-product. The regression equation parameter solution formula is as follows:

然后采用外标法,根据标准样品曲线计算样品中α-甲基苯乙烯、苯乙酮和枯基醇的浓度。公式如下:Then, the external standard method is used to calculate the concentrations of α-methylstyrene, acetophenone and cumyl alcohol in the sample according to the standard sample curve. The formula is as follows:

其中,ci表示交联副产物i(包括α-甲基苯乙烯、苯乙酮和枯基醇)的浓度,单位为mg/g;ki表示交联副产物i标准曲线的斜率,单位为mg;mj表示第j个样品的质量,单位为g;Aji表示第j个样品中交联副产物i的峰面积,无单位。Wherein, ci represents the concentration of cross-linked by-product i (including α-methylstyrene, acetophenone and cumyl alcohol), in mg/g; ki represents the slope of the standard curve of cross-linked by-product i, in mg; mj represents the mass of the j-th sample, in g; Aji represents the peak area of cross-linked by-product i in the j-th sample, without unit.

表1110kVXLPE绝缘电缆规格参数Table 1110kV XLPE insulated cable specifications

表2标准浓度溶液Table 2 Standard concentration solutions

不同祛气时间的样品测试结果如图7所示,本发明实现对XLPE样品的交联副产物成分及含量能够准确定量,得到α-甲基苯乙烯、苯乙酮、枯基醇三种交联副产物在XLPE绝缘中的浓度,使对高压电缆祛气效果的评估更准确高效。The test results of samples with different degassing times are shown in FIG7 . The present invention can accurately quantify the composition and content of the cross-linked by-products of the XLPE sample, and obtain the concentrations of the three cross-linked by-products, namely, α-methylstyrene, acetophenone, and cumyl alcohol, in the XLPE insulation, so that the evaluation of the degassing effect of the high-voltage cable is more accurate and efficient.

以上实施例的说明只是用于帮助理解本发明的技术方案及其核心思想,应当指出,对于本技术领域的技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。The description of the above embodiments is only used to help understand the technical solution and core ideas of the present invention. It should be pointed out that for technicians in this technical field, several improvements and modifications can be made to the present invention without departing from the principles of the present invention. These improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims (9)

1.一种不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量的测试方法,其特征在于,包括如下步骤:1. A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and time conditions, characterized in that it comprises the following steps: S1、将电缆试样去除导体和半导电尼龙带、半导电多特带部分,保留导体屏蔽、XLPE绝缘和绝缘屏蔽三个部分;S1. Remove the conductor, semi-conductive nylon tape and semi-conductive multi-tape parts from the cable sample, and keep the conductor shield, XLPE insulation and insulation shield; S2、将电缆试样分为两组,分别对电缆试样进行热处理;S2. Divide the cable samples into two groups and perform heat treatment on the cable samples respectively; S3、将热处理后的电缆试样进一步切割,分别切取包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品以及XLPE绝缘的内层、中层和外层样品;S3, further cutting the heat-treated cable sample to obtain the whole cable sample including the conductor shield, XLPE insulation, insulation shield, and the inner layer, middle layer and outer layer samples of the XLPE insulation; S4、将电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品进行热处理;S4, heat treating the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation; S5、利用枯基醇、苯乙酮和α-甲基苯乙烯三种分析测试标准品,配置不同浓度的标准溶液,利用气相色谱-质谱联用法,对不同浓度的标准溶液进行分析测试,得到标准溶液中枯基醇、苯乙酮、α-甲基苯乙烯三种交联副产物的峰面积与质量的线性关系;S5. Using three analytical test standards, namely, cumyl alcohol, acetophenone and α-methylstyrene, standard solutions of different concentrations are prepared, and the standard solutions of different concentrations are analyzed and tested by gas chromatography-mass spectrometry to obtain a linear relationship between the peak area and mass of the three cross-linking byproducts of cumyl alcohol, acetophenone and α-methylstyrene in the standard solution; S6、利用气相色谱-质谱联用法,对步骤S4热处理后的电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品分别进行分析测试,将样品测试中测得的三种交联副产物的峰面积带入此线性关系,得到三种交联副产物在绝缘样品中的浓度。S6. Using gas chromatography-mass spectrometry, the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation after the heat treatment in step S4 are analyzed and tested respectively, and the peak areas of the three cross-linked by-products measured in the sample test are brought into this linear relationship to obtain the concentrations of the three cross-linked by-products in the insulation sample. 2.根据权利要求1所述的测试方法,其特征在于,步骤S2具体包括如下步骤:2. The testing method according to claim 1, characterized in that step S2 specifically comprises the following steps: S21、将样品分成两组,每组若干段样品,分别标号A、B;S21, divide the samples into two groups, each group has several sections of samples, labeled A and B respectively; S22、A、B两组各保留一个样品,将其他样品置于恒温箱进行模拟祛气,两组A、B热处理的温度分别设定65℃和70℃,每间隔12h取样一次,祛气周期为144h。One sample was retained from each of the two groups S22, A, and B, and the other samples were placed in a constant temperature box for simulated degassing. The heat treatment temperatures of the two groups A and B were set at 65°C and 70°C, respectively. Sampling was taken every 12 hours, and the degassing cycle was 144 hours. 3.根据权利要求1所述的测试方法,其特征在于,步骤S3的具体步骤为:用电缆切割机切取扇形的包含导体屏蔽、XLPE绝缘、绝缘屏蔽的电缆整体样品,得到电缆整体样品;制取XLPE绝缘的内层、中层和外层样品时,在电缆整体样品的基础上,去除导体屏蔽、绝缘屏蔽,剩下XLPE绝缘部分,然后平行于弧面切成三等份,由内向外分别为XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品。3. The testing method according to claim 1 is characterized in that the specific steps of step S3 are: using a cable cutter to cut a fan-shaped cable sample including a conductor shield, XLPE insulation, and insulation shield to obtain a cable sample; when preparing the inner, middle and outer layer samples of XLPE insulation, on the basis of the cable sample, the conductor shield and insulation shield are removed, leaving the XLPE insulation part, and then cut into three equal parts parallel to the arc surface, which are the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation from the inside to the outside. 4.根据权利要求1所述的测试方法,其特征在于,步骤S4的具体步骤为:将电缆整体样品、XLPE绝缘的内层、XLPE绝缘的中层和XLPE绝缘的外层样品分装在顶空瓶中,利用恒温热烘箱进行热处理,热处理的条件是:加热温度120℃,加热时间5h。4. The testing method according to claim 1 is characterized in that the specific steps of step S4 are: the whole cable sample, the inner layer of XLPE insulation, the middle layer of XLPE insulation and the outer layer of XLPE insulation are packed in headspace bottles, and heat-treated in a constant temperature oven, and the heat treatment conditions are: heating temperature 120° C., heating time 5 h. 5.根据权利要求1所述的测试方法,其特征在于,步骤S5中:将枯基醇分别配置成0.2mg/mL、0.4mg/mL、1.0mg/mL、2.0mg/mL、4.0mg/mL、20.0mg/mL 6种不同浓度的标准溶液,苯乙酮分别配置成0.3mg/mL、0.6mg/mL、1.5mg/mL、3.0mg/mL、6.0mg/mL、30.0mg/mL 6种不同浓度的标准溶液,α-甲基苯乙烯分别配置成0.02mg/mL、0.04mg/mL、0.1mg/mL、0.2mg/mL、0.4mg/mL、2.0mg/mL 6种不同浓度的标准溶液。5. The test method according to claim 1, characterized in that in step S5: cumyl alcohol is respectively configured into 6 standard solutions of different concentrations of 0.2 mg/mL, 0.4 mg/mL, 1.0 mg/mL, 2.0 mg/mL, 4.0 mg/mL, and 20.0 mg/mL, acetophenone is respectively configured into 6 standard solutions of different concentrations of 0.3 mg/mL, 0.6 mg/mL, 1.5 mg/mL, 3.0 mg/mL, 6.0 mg/mL, and 30.0 mg/mL, and α-methylstyrene is respectively configured into 6 standard solutions of different concentrations of 0.02 mg/mL, 0.04 mg/mL, 0.1 mg/mL, 0.2 mg/mL, 0.4 mg/mL, and 2.0 mg/mL. 6.根据权利要求1或5所述的测试方法,其特征在于,步骤S5具体包括如下步骤:6. The testing method according to claim 1 or 5, characterized in that step S5 specifically comprises the following steps: S51、用气相色谱质谱联用仪检测样品与6种不同浓度的标准溶液,得到每一种交联副产物在6种不同浓度下的峰面积,将6个测试数据与原点记录在坐标平面上,拟合出每一种交联副产物对应的回归方程y=kx+b,其中纵坐标y代表交联副产物质量,横坐标x代表交联副产物峰面积,回归方程参数求解公式如下:S51. Use gas chromatography-mass spectrometry to detect the sample and 6 standard solutions of different concentrations, obtain the peak area of each cross-linked by-product at 6 different concentrations, record the 6 test data and the origin on the coordinate plane, and fit the regression equation y=kx+b corresponding to each cross-linked by-product, where the ordinate y represents the mass of the cross-linked by-product, and the abscissa x represents the peak area of the cross-linked by-product. The regression equation parameter solution formula is as follows: 7.根据权利要求1所述的测试方法,其特征在于,步骤S6具体包括如下步骤:7. The testing method according to claim 1, characterized in that step S6 specifically comprises the following steps: S61、采用外标法,根据交联副产物峰面积与质量的关系曲线,计算样品中各种交联副产物的浓度,公式如下:S61. Using the external standard method, the concentration of various cross-linking by-products in the sample is calculated based on the relationship curve between the peak area and mass of the cross-linking by-products. The formula is as follows: 其中,ci表示交联副产物i的浓度,i包括α-甲基苯乙烯、苯乙酮和枯基醇,单位为mg/g;ki表示交联副产物i标准曲线的斜率,单位为mg;mj表示第j个样品的质量,单位为g;Aji表示第j个样品中交联副产物i的峰面积,无单位。Wherein, ci represents the concentration of cross-linked by-product i, i includes α-methylstyrene, acetophenone and cumyl alcohol, and the unit is mg/g; ki represents the slope of the standard curve of cross-linked by-product i, and the unit is mg; mj represents the mass of the j-th sample, and the unit is g; Aji represents the peak area of cross-linked by-product i in the j-th sample, and the unit is unitless. 8.根据权利要求1所述的测试方法,其特征在于,步骤S5或S6所述的气相色谱-串联质谱法检测条件:色谱柱为HP-INNOWax,规格为30m×0.25mm×0.25μm;进样口温度为250℃;升温程序:初始温度40℃,保持3min,以10℃/min升温至250℃,保持5min;8. The test method according to claim 1, characterized in that the gas chromatography-tandem mass spectrometry detection conditions described in step S5 or S6 are: the chromatographic column is HP-INNOWax, with a specification of 30m×0.25mm×0.25μm; the injection port temperature is 250°C; the heating program is: initial temperature 40°C, maintained for 3min, heated to 250°C at 10°C/min, and maintained for 5min; 所用载气为纯度为99.9995%的氦气,氦气流速为1mL/min;进样方式为分流进样,分流比30:1,进样量为100μL;质谱采集方式为scan模式,m/z范围是33-500。The carrier gas used was helium with a purity of 99.9995% and a helium flow rate of 1 mL/min; the injection method was split injection with a split ratio of 30:1 and an injection volume of 100 μL; the mass spectrometry acquisition method was scan mode with an m/z range of 33-500. 9.权利要求1所述的测试方法在测试不同祛气温度和时间条件下的高压XLPE电缆绝缘内部交联副产物含量中的应用。9. Application of the test method described in claim 1 in testing the content of cross-linking byproducts inside the insulation of high-voltage XLPE cables under different degassing temperature and time conditions.
CN202410929748.3A 2024-07-11 2024-07-11 A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times Pending CN118777459A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202410929748.3A CN118777459A (en) 2024-07-11 2024-07-11 A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202410929748.3A CN118777459A (en) 2024-07-11 2024-07-11 A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times

Publications (1)

Publication Number Publication Date
CN118777459A true CN118777459A (en) 2024-10-15

Family

ID=92985724

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202410929748.3A Pending CN118777459A (en) 2024-07-11 2024-07-11 A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times

Country Status (1)

Country Link
CN (1) CN118777459A (en)

Similar Documents

Publication Publication Date Title
CN103245519B (en) The device of the assessment of transformer oil Aging of Oil-paper Insulation in Oil and life prediction and Forecasting Methodology thereof
CN106645468A (en) Method for measuring VOCs in packaging material by virtue of gas chromatography-mass spectrometry
Bruzzoniti et al. GC methods for the determination of methanol and ethanol in insulating mineral oils as markers of cellulose degradation in power transformers
CN105510469B (en) The detection method of furfural content in a kind of transformer insulating paper
CN104215732A (en) Method of taking Tenax as simulant to measure migration amount from paper and volatile and semi-volatile organic matter in paperboard by TD-GC/MS
Chen et al. Study on aging assessment model of transformer cellulose insulation paper based on methanol in oil
CN112114072A (en) Detection method for simultaneously analyzing multiple organic gases
EP3188201B1 (en) Method for inspecting oil-filled electrical apparatus
JP2024138113A (en) Data for quantitative analysis of brominated flame retardant compounds
CN101101279A (en) Quantitative analysis method for battery electrolyte organic components
CN102788856B (en) The analytical approach of elementary sulfur quantitative and qualitative analysis in liquefied petroleum gas (LPG)
CN106248912A (en) A kind of characterizing method of transformer oil ageing
CN118777459A (en) A method for testing the content of cross-linked byproducts in high-voltage XLPE cable insulation under different degassing temperatures and times
Beiner et al. Oddy tests: Adding the analytical dimension
Chen et al. An improved method of detection and concentration of methanol in oil-paper insulation
KR20110139968A (en) Sample analysis device and sample analysis method
CN113504333A (en) Method for detecting organic matter migration amount in paper packaging material
Cao et al. QSRR study of GC retention indices of volatile compounds emitted from Mosla chinensis Maxim by multiple linear regression
CN115469037B (en) A method for detecting the content of rubber antioxidant in transformer oil
CN116699040A (en) An analysis method and database of key odor components in packaged printed matter
Pacenti et al. New automated and high‐throughput quantitative analysis of urinary ketones by multifiber exchange‐solid phase microextraction coupled to fast gas chromatography/negative chemical‐electron ionization/mass spectrometry
Chen et al. The application research of solid‐phase extraction and headspace gas chromatography in the detection of methanol in transformer oil
Żuchowska et al. Protocol for the untargeted analysis of volatile metabolites in the headspace of biological samples using Thin-Film Microextraction coupled to GC–MS
Roger et al. An alternative method for irones quantification in iris rhizomes using headspace solid‐phase microextraction
CN111551663B (en) Quantitative method for determining soil fatty acid methyl ester and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination