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CN105300978A - Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent - Google Patents

Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent Download PDF

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CN105300978A
CN105300978A CN201510795457.0A CN201510795457A CN105300978A CN 105300978 A CN105300978 A CN 105300978A CN 201510795457 A CN201510795457 A CN 201510795457A CN 105300978 A CN105300978 A CN 105300978A
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warm
clear liquid
color
detection method
warm mix
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CN105300978B (en
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柳浩�
杨炎生
王真
杨丽英
李恩光
李宁
董雨明
李振
徐世法
索智
许鹰
金珊珊
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BEIJING ZHENGDA KUNSHUN TECHNOLOGY TESTING CO LTD
Beijing Municipal Road & Bridge Building Material Group Co ltd
Beijing University of Civil Engineering and Architecture
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BEIJING ZHENGDA KUNSHUN TECHNOLOGY TESTING CO LTD
Beijing Municipal Road & Bridge Building Material Group Co ltd
Beijing University of Civil Engineering and Architecture
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02A30/00Adapting or protecting infrastructure or their operation
    • Y02A30/30Adapting or protecting infrastructure or their operation in transportation, e.g. on roads, waterways or railways

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Abstract

本发明涉及一种温拌沥青中含油溶性胺类表面活性剂温拌剂检测方法,包括以下步骤:(1)称取待测样品,并加入溶剂,加热至溶剂呈微沸状态且颜色变为浅黄色;(2)将步骤(1)中的上层清液倒出,并滴入检测试剂,观察清液的颜色变化;(3)将步骤(1)中的上层清液倒出,并加热清液,然后滴入检测试剂,观察清液的颜色变化,(4)根据步骤(2)和步骤(3)判断待测样品中是否含有油溶性胺类表面活性剂型温拌剂。本发明中的显色反应检测方法对试验仪器、设备及检测人员要求不高,检测成本低,灵敏度较高,具有较高的实用价值。The invention relates to a method for detecting an oil-soluble amine surfactant warm mix agent in warm mix asphalt, comprising the following steps: (1) weighing a sample to be tested, adding a solvent, and heating until the solvent is slightly boiling and the color changes to light yellow; (2) pour out the supernatant in step (1), and drop into the detection reagent, observe the color change of the supernatant; (3) pour out the supernatant in step (1), and heat clear liquid, then drip detection reagent, observe the color change of clear liquid, (4) judge whether to contain oil-soluble amine surfactant type warm mixing agent in the sample to be tested according to step (2) and step (3). The color reaction detection method in the present invention has low requirements on test instruments, equipment and test personnel, low test cost, high sensitivity and high practical value.

Description

一种温拌沥青中含油溶性胺类表面活性剂温拌剂检测方法A detection method for warm mix agent containing oil-soluble amine surfactant in warm mix asphalt

技术领域technical field

本发明属于公路沥青路面温拌技术领域,具体涉及一种温拌沥青中含油溶性胺类表面活性剂温拌剂检测方法。The invention belongs to the technical field of warm mixing of highway asphalt pavement, and in particular relates to a detection method for a warm mixing agent containing an oil-soluble amine surfactant in warm mixing asphalt.

背景技术Background technique

温拌沥青路面材料由于其低碳环保和节能减排的优点而得到了广泛的关注和应用。目前,市场上常用的是基于表面活性剂型温拌剂的温拌沥青路面材料,其发展到现在已至第三代,它是将一种油溶性胺类表面活性剂型温拌剂加入沥青后,经过一定的加工工艺,形成质量稳定的、可降低沥青拌和、施工温度的产品。其在使用过程中大大简化了生产工艺,不需要对现有拌和设备进行改造,降低了对设备的依赖性;同时,大规模的工业化生产使其质量变异性大大降低,对沥青及沥青混合料的路用性能起到了保障。Warm mix asphalt pavement material has been widely concerned and applied due to its advantages of low carbon, environmental protection, energy saving and emission reduction. At present, warm mix asphalt pavement materials based on surfactant-type warm mix agent are commonly used in the market. It has been developed to the third generation. After a certain processing technology, a product with stable quality can be formed, which can reduce the temperature of asphalt mixing and construction. It greatly simplifies the production process in the process of use, does not need to modify the existing mixing equipment, and reduces the dependence on the equipment; at the same time, the large-scale industrial production greatly reduces the quality variability, and the asphalt and asphalt mixture The road performance is guaranteed.

目前温拌沥青中温拌剂是否存还没有检测方法,温拌沥青的相关技术规范还没有制定出来,无法对其进行质量监管和控制,因此为有效对温拌沥青中的温拌剂进行检测,提供一种检测迅速、便捷的检测方法具有十分重要的意义。At present, there is no detection method for the existence of warm mix agent in warm mix asphalt, and the relevant technical specifications of warm mix asphalt have not been formulated, so it is impossible to supervise and control its quality. Therefore, in order to effectively detect the warm mix agent in warm mix asphalt, It is of great significance to provide a rapid and convenient detection method.

发明内容Contents of the invention

本发明是利用温拌剂与溴酚蓝指示剂发生化学反应后溶液呈现蓝色的现象来定性检测温拌沥青中是否存在温拌剂,该方法简单易行,解决了当前温拌沥青中温拌剂没有方法检测的问题。The present invention uses the phenomenon that the solution turns blue after the chemical reaction between the warm mix agent and the bromophenol blue indicator to qualitatively detect whether the warm mix agent exists in the warm mix asphalt. There is no way to detect the agent.

本发明的技术方案如下:Technical scheme of the present invention is as follows:

一种温拌沥青中含油溶性胺类表面活性剂温拌剂检测方法,包括以下步骤:A kind of warm mix agent detection method containing oil-soluble amine surfactant in warm mix asphalt, comprises the following steps:

(1)称取待测样品,并加入溶剂,加热至溶剂呈微沸状态且颜色变为浅黄色;(1) Weigh the sample to be tested, add solvent, and heat until the solvent is slightly boiling and the color turns light yellow;

(2)将步骤(1)中的上层清液倒出,并滴入检测试剂,观察清液的颜色变化;(2) Pour out the supernatant in step (1), and drop into the detection reagent, observe the color change of the supernatant;

(3)将步骤(1)中的上层清液倒出,并加热清液,然后滴入检测试剂,观察清液的颜色变化,(3) Pour out the supernatant in step (1), and heat the supernatant, then drip the detection reagent, observe the color change of the supernatant,

(4)根据步骤(2)和步骤(3)判断待测样品中是否含有油溶性胺类表面活性剂型温拌剂,(4) judge according to step (2) and step (3) whether contain oil-soluble amine surfactant type warm mixing agent in the sample to be tested,

所述检测试剂为溶于中性有机溶剂中的溴酚蓝指示剂。The detection reagent is a bromophenol blue indicator dissolved in a neutral organic solvent.

所述检测试剂为由以下组分组成:10~100ml异丙醇,0.02~3.0g溴酚蓝。The detection reagent is composed of the following components: 10-100ml of isopropanol and 0.02-3.0g of bromophenol blue.

优选的,所述的异丙醇为分析纯。Preferably, the isopropanol is analytically pure.

优选的,所述步骤(1)中待测样品的加入量为0.1-2.0g;溶剂的加入量为:10-200ml。Preferably, the added amount of the sample to be tested in the step (1) is 0.1-2.0 g; the added amount of the solvent is: 10-200 ml.

优选的,所述步骤(1)中的溶剂为异丙醇。Preferably, the solvent in the step (1) is isopropanol.

优选的,所述步骤(2)中检测试剂的加入量为3-5滴。Preferably, the amount of detection reagent added in the step (2) is 3-5 drops.

优选的,所述步骤(3)中的加热时间为1-3min,检测试剂的加入量为3-5滴。Preferably, the heating time in the step (3) is 1-3 min, and the amount of detection reagent added is 3-5 drops.

优选的,所述的步骤(4)中待测样品中是否含有油溶性胺类表面活性剂型温拌剂为:步骤(2)中的清液颜色变为蓝色,且步骤(3)中清液颜色变为亮黄色表示待测样品中含有温拌剂;若步骤(2)中的清液颜色变蓝色,步骤(3)中清液颜色也变为蓝色,表示待测样品中不含温拌剂;若步骤(2)中清液不变色或出现非蓝色的改变(包括浅绿色、墨绿等)表示待测样品中不含温拌剂。Preferably, whether oil-soluble amine surfactant type warm mixing agent is contained in the sample to be tested in the described step (4) is: the color of the clear liquid in the step (2) turns blue, and the clear liquid in the step (3) The color of the solution turns bright yellow to indicate that the sample to be tested contains warm mixing agent; if the color of the clear solution in step (2) turns blue, the color of the clear solution in step (3) also turns blue, indicating that there is no Contains a warming agent; if the clear liquid does not change color or changes in non-blue color (including light green, dark green, etc.) in step (2), it means that the sample to be tested does not contain a warming agent.

本发明的原理是萃取和指示剂显色:用异丙醇把温拌沥青中的温拌剂萃取出来,加热有助于加速这个过程,然后指示剂与温拌剂发生反应生成蓝色的物质,所以清液变为蓝色;当然这个过程中也会把沥青中溶于异丙醇中的物质萃取出来,呈现黄色的物质是沥青中的一些组分,即便不含温拌剂,沥青本身加入异丙醇加热也会呈现变黄色这一现象,指示剂检测的物质在异丙醇中是透明无色的。The principle of the present invention is extraction and indicator color development: use isopropanol to extract the warm mix agent in the warm mix asphalt, heating helps to accelerate this process, and then the indicator reacts with the warm mix agent to form a blue substance , so the clear liquid turns blue; of course, this process will also extract the substances dissolved in isopropanol in the asphalt, and the yellow substances are some components in the asphalt, even if there is no warm mix agent, the asphalt itself Adding isopropanol and heating will also show the phenomenon of yellowing, and the substance detected by the indicator is transparent and colorless in isopropanol.

直接添加指示剂会导致指示剂用量过大,指示剂的颜色会干扰颜色的判断,影响检测结果;指示剂用溶剂稀释的目的就是把其浓度降低,即使这样,在使用的时候其用量也不能过多,最多也不过5滴,否则影响检测结果。Adding the indicator directly will lead to an excessive amount of the indicator, and the color of the indicator will interfere with the judgment of the color and affect the test result; the purpose of diluting the indicator with a solvent is to reduce its concentration. Too much, no more than 5 drops, otherwise it will affect the test results.

因此步骤(1)中微沸呈浅黄色,说明加热时间不长(若加热时间过长,沥青中的深颜色物质也会被萃取出来,从而干扰颜色的判断),这样萃取出来温拌剂的量较少,而温拌剂具有一定的挥发性,步骤(3)中清液经过长时间持续加热,温拌剂挥发出来,因此指示剂加入后仅是指示剂颜色和清液颜色叠加后的颜色。Therefore, the slight boiling in step (1) turns light yellow, indicating that the heating time is not long (if the heating time is too long, the dark-colored substances in the asphalt will also be extracted, thereby interfering with the judgment of the color), so that the extracted warm mix agent The amount is less, and the warm mixing agent has a certain volatility. In step (3), the clear liquid is continuously heated for a long time, and the warm mixing agent is volatilized. Therefore, after the indicator is added, only the color of the indicator and the color of the clear liquid are superimposed. color.

本发明的有益效果如下:The beneficial effects of the present invention are as follows:

1本发明提供了温拌沥青中温拌剂是否存在的检测方法。1 The present invention provides a detection method for the presence of warm mix agent in warm mix asphalt.

2本发明中对实验仪器、设备及检测人员要求不高,检测成本低,具有较高的实用价值。2. In the present invention, the requirements for experimental instruments, equipment and testing personnel are not high, the testing cost is low, and it has high practical value.

3发明人已对检测方法进行了大量数据的测定,该检测方法使用情况良好,说明本发明试验方法是合理的、可靠的、实用的.3 The inventor has carried out the measurement of a large amount of data to the detection method, and this detection method is in good use, indicating that the test method of the present invention is reasonable, reliable and practical.

具体实施方式detailed description

下面结合具体实施方式对本发明做进一步说明。The present invention will be further described below in combination with specific embodiments.

实施例1Example 1

一种温拌沥青中温拌剂检测试剂,由包括以下重量份的组分组成A detection reagent for warm mix agent in warm mix asphalt, consisting of the following components in parts by weight

异丙醇(100ml),溴酚蓝:0.2g。Isopropanol (100ml), bromophenol blue: 0.2g.

采用上述的温拌沥青中温拌剂检测试剂对某种温拌沥青进行检测,包括以下步骤:Using the above warm mix agent detection reagent in warm mix asphalt to detect a certain kind of warm mix asphalt, including the following steps:

(1)称取1g温拌沥青于烧杯中,然后加入50ml异丙醇,加热至异丙醇呈微沸状态且颜色变为浅黄色;(1) Weigh 1g of warm-mix asphalt into a beaker, then add 50ml of isopropanol, and heat until the isopropanol is slightly boiling and the color turns light yellow;

(2)将步骤(1)中的上层清液倒出,并加入5滴检测试剂,观察清液的颜色变化,清液颜色变为蓝色;(2) Pour out the supernatant in step (1), and add 5 drops of detection reagent, observe the color change of the supernatant, and the color of the supernatant turns blue;

(3)将步骤(1)中的上层清液倒出,并加热煮沸清液,保持沸腾状态2min,然后滴入检测试剂,观察清液的颜色变化,清液颜色变为亮黄色;(3) Pour out the supernatant in step (1), heat and boil the clear liquid, keep boiling for 2 minutes, then drop in the detection reagent, observe the color change of the clear liquid, and the color of the clear liquid becomes bright yellow;

(4)表示待测样品中含有温拌剂。(4) indicates that the sample to be tested contains a warm mixing agent.

结论:与加有油溶性胺类表面活性剂型温拌剂的事实相符。Conclusion: It is consistent with the fact that oil-soluble amine surfactant type warm mixing agent is added.

实施例2Example 2

一种温拌沥青中温拌剂检测试剂,由包括以下重量份的组分组成A detection reagent for warm mix agent in warm mix asphalt, consisting of the following components in parts by weight

异丙醇(100ml),溴酚蓝:0.3g。Isopropanol (100ml), bromophenol blue: 0.3g.

采用上述的温拌沥青中温拌剂检测试剂对某种温拌沥青进行检测,包括以下步骤:Using the above warm mix agent detection reagent in warm mix asphalt to detect a certain kind of warm mix asphalt, including the following steps:

(1)称取0.5g温拌沥青于烧杯中,然后加入40ml异丙醇,加热至异丙醇呈微沸状态且颜色变为浅黄色;(1) Weigh 0.5g of warm-mix asphalt into a beaker, then add 40ml of isopropanol, and heat until the isopropanol is slightly boiling and the color turns light yellow;

(2)将步骤(1)中的上层清液倒出,并加入5滴检测试剂,观察清液的颜色变化,清液颜色变为蓝色;(2) Pour out the supernatant in step (1), and add 5 drops of detection reagent, observe the color change of the supernatant, and the color of the supernatant turns blue;

(3)将步骤(1)中的上层清液倒出,并加热煮沸清液,保持沸腾状态1min,然后滴入检测试剂,观察清液的颜色变化,清液颜色变为蓝色;(3) Pour out the supernatant in step (1), heat and boil the clear liquid, keep boiling for 1 min, then drop in the detection reagent, observe the color change of the clear liquid, and the clear liquid turns blue;

(4)表示待测样品中不含温拌剂。(4) means that the sample to be tested does not contain warm mixing agent.

结论:与不加有油溶性胺类表面活性剂型温拌剂的事实相符。Conclusion: It is consistent with the fact that oil-soluble amine surfactant type warm mixing agent is not added.

实施例3Example 3

一种温拌沥青中温拌剂检测试剂,由包括以下重量份的组分组成A detection reagent for warm mix agent in warm mix asphalt, consisting of the following components in parts by weight

异丙醇(50ml),溴酚蓝:0.08g。Isopropanol (50ml), bromophenol blue: 0.08g.

采用上述的温拌沥青中温拌剂检测试剂对某种温拌沥青进行检测,包括以下步骤:Using the above warm mix agent detection reagent in warm mix asphalt to detect a certain kind of warm mix asphalt, including the following steps:

(1)称取1.5g温拌沥青于烧杯中,然后加入50ml异丙醇,加热至异丙醇呈微沸状态且颜色变为浅黄色;(1) Weigh 1.5g of warm-mix asphalt into a beaker, then add 50ml of isopropanol, and heat until the isopropanol is slightly boiling and the color turns light yellow;

(2)将步骤(1)中的上层清液倒出,并加入5滴检测试剂,观察清液的颜色变化,清液颜色变为亮黄色。(2) Pour out the supernatant in step (1), add 5 drops of detection reagent, observe the color change of the supernatant, and the color of the supernatant turns bright yellow.

(3)表示待测样品中不含温拌剂。(3) means that the sample to be tested does not contain warm mixing agent.

结论:与不加有油溶性胺类表面活性剂型温拌剂的事实相符。Conclusion: It is consistent with the fact that oil-soluble amine surfactant type warm mixing agent is not added.

Claims (8)

1. a containing oil soluble amine surfactants warm-mixing agent detection method in warm-mixed asphalt, comprises the following steps:
(1) take testing sample, and add solvent, be heated to solvent and be slight boiling condition and color becomes light yellow;
(2) supernatant liquor in step (1) is poured out, and instillation detects reagent, observe the color change of clear liquid;
(3) poured out by the supernatant liquor in step (1), and heat clear liquid, then instillation detects reagent, observes the color change of clear liquid,
(4) judge whether containing oil-soluble amine surfactant type warm-mixing agent in testing sample according to step (2) and step (3),
Described detection reagent is the bromophenol blue indicator be dissolved in neutral organic solvent.
2. detection method according to claim 1, described detection reagent is composed of the following components: 10 ~ 100ml isopropyl alcohol, 0.02 ~ 3.0g bromophenol blue.
3. detection method according to claim 2, described isopropyl alcohol is pure for analyzing.
4. detection method according to claim 1, in described step (1), the addition of testing sample is 0.1-2.0g; The addition of solvent is: 10-200ml.
5. detection method according to claim 4, the solvent in described step (1) is isopropyl alcohol.
6. detection method according to claim 2, the addition detecting reagent in described step (2) is that 3-5 drips.
7. detection method according to claim 6, the heat time in described step (3) is 1-3min, and the addition detecting reagent is that 3-5 drips.
8. detection method according to claim 1, in described step (4) in testing sample containing oil-soluble amine surfactant type warm-mixing agent be whether: the clear liquid color in step (2) becomes blueness, and in step (3), clear liquid color becomes glassy yellow and represents in testing sample containing warm-mixing agent; If the clear liquid color in step (2) becomes blue, in step (3), clear liquid color also becomes blueness, represents in testing sample not containing warm-mixing agent; If clear liquid nondiscolouring or occur that the change of non-blueness represents in testing sample not containing warm-mixing agent in step (2).
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105806747A (en) * 2016-02-24 2016-07-27 北京建筑大学 Asphalt-aggregate interface adhesion property testing method
CN114062352A (en) * 2020-08-04 2022-02-18 中国石油天然气股份有限公司 Method for identifying warm mixing agent containing amine surfactant in asphalt

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