CN103994947A - Fiber specific gravity testing method - Google Patents
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- 238000012360 testing method Methods 0.000 title claims abstract description 23
- 230000005484 gravity Effects 0.000 title abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000012153 distilled water Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 10
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- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims 2
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- 230000008901 benefit Effects 0.000 description 2
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- 239000008188 pellet Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种快速测试纤维比重的方法。The invention relates to a method for rapidly testing fiber specific gravity.
背景技术Background technique
密度是表征纤维物理性能的一个重要的参数,其测试方法始终为广大学者所关注,并进行了多方面的探索和研究,提出了许多测试方法,如专利CN103091201提出了一种利用纤维质量分析仪测定纸浆纤维粒子的纤维密度测定方法;又如专利CN103323360提出了利用密度梯度法测定一种纤维素纤维混纺产品的密度,进而计算纤维含量测定方法及装置。概括起来,目前被国际标准化组织承认,并列入相关标准的试验方法有三种:液体置换法、沉浮法、密度梯度柱法。但均因纤维集合体中含有大量空气,干扰测试结果,大大制约了其使用范围,致使到目前仍无有效和快速的测试纤维比重的方法。在这三种测定方法中,主要存在以下几方面的问题:(1)实验过程中,附着在纤维表面和纤维单丝间夹杂气泡的存在使数据误差较大,如何去除气泡比较麻烦,三种测试方法都存在这方面的问题;(2)需要解决纤维表面张力效应和温度变化对密度测定的影响;(3)必须准确选用各方法中浸润液所需的溶液,对于浸润液的密度精度和密度范围要求很大,产生的误差比较大;(4)需要对纤维悬浮态作出正确的判定,该过程中人为的误差很大,实验测试的数据误差很大,精度不高;(5)配置密度梯度柱的过程是一个非常繁琐的过程,因为配置的密度梯度柱自上而下的密度并不一定成线性,实验过程耗时长,且对于纤维悬浮态的判定存在人为的误差。而且纤维小球的取样量只有毫克级,太小。另外,对纤维小球的脱泡方法也有缺陷,脱泡不彻底。Density is an important parameter to characterize the physical properties of fibers. Its test method has always been concerned by scholars, and many explorations and researches have been carried out, and many test methods have been proposed. For example, the patent CN103091201 proposed a fiber quality analyzer. A fiber density measurement method for measuring pulp fiber particles; another example is the patent CN103323360, which proposes a method and device for measuring the density of a cellulose fiber blended product by using a density gradient method, and then calculating the fiber content. To sum up, there are currently three test methods recognized by the International Organization for Standardization and included in relevant standards: liquid displacement method, sink-float method, and density gradient column method. However, because the fiber aggregate contains a large amount of air, which interferes with the test results and greatly restricts its scope of use, there is still no effective and fast method for testing the specific gravity of fibers so far. In these three measurement methods, there are mainly the following problems: (1) During the experiment, the presence of air bubbles attached to the surface of the fiber and between the fiber monofilaments makes the data error larger, and how to remove the air bubbles is more troublesome. There are problems in this aspect in all test methods; (2) It is necessary to solve the influence of fiber surface tension effect and temperature change on the density measurement; (3) the solution required for the immersion solution in each method must be accurately selected, and the density accuracy of the immersion solution and The density range is required to be very large, and the resulting error is relatively large; (4) It is necessary to make a correct judgment on the fiber suspension state. In this process, the human error is very large, the experimental test data has a large error, and the accuracy is not high; (5) Configuration The process of the density gradient column is a very cumbersome process, because the top-to-bottom density of the configured density gradient column is not necessarily linear, the experimental process takes a long time, and there are artificial errors in the judgment of the fiber suspension state. Moreover, the sampling amount of the fiber pellets is only at the milligram level, which is too small. In addition, the defoaming method for fiber pellets is also defective, and the defoaming is not thorough.
发明内容Contents of the invention
针对现有技术存在的不足,本发明所要解决的技术问题是,提供一种操作简单,测试效率高,测试精度高,可用于大量快速的测定各种纤维密度的测定的纤维比重的测试方法。Aiming at the deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a test method with simple operation, high test efficiency and high test accuracy, which can be used for a large number of rapid determination of fiber specific gravity for the determination of various fiber densities.
为解决上述技术问题,本发明所采取的技术方案是:一种纤维比重的测试方法,包括如下步骤:In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a kind of test method of fiber specific gravity, comprises the steps:
一、仅装有水的比重瓶质量W1的测量:1. Measurement of the mass W 1 of a pycnometer filled with water only:
(1)、将灌满蒸馏水的100ml比重瓶放入盛有蒸馏水的150ml烧杯中,并且保持烧杯中的蒸馏水没过比重瓶0.1~1cm;(1), put the 100ml pycnometer filled with distilled water into a 150ml beaker filled with distilled water, and keep the distilled water in the beaker submerged by 0.1-1cm of the pycnometer;
(2)、然后将烧杯连同比重瓶放入抽真空装置中抽真空,控制真空度达到99.5%~99.9%,并保持0.5~3h;(2), then put the beaker together with the pycnometer into a vacuum device to evacuate, control the vacuum degree to 99.5% to 99.9%, and keep it for 0.5 to 3 hours;
(3)然后将比重瓶取出放入密封罐中至于20℃条件下平衡24h后称其质量,即得比重瓶+水的质量W1;(3) then take out the pycnometer and put it in a sealed tank, balance it for 24h under the condition of 20°C and weigh its quality, then get the quality W of the pycnometer+water;
二、纤维质量W2的测量:2. Measurement of fiber quality W 2 :
(4)、取待测定纤维20g,用无水酒精或乙醚浸泡纤维20min~50min,去除纤维表面的油剂,然后在50℃~120℃环境中烘干时间在1h~3h;(4) Take 20g of the fiber to be measured, soak the fiber with absolute alcohol or ether for 20-50 minutes, remove the oil on the surface of the fiber, and then dry it in an environment of 50°C-120°C for 1h-3h;
(5)、干燥完毕后用电子天平称量纤维的质量,标记为W2;(5), after drying, weigh the quality of fiber with electronic balance, marked as W 2 ;
三、装有纤维和水的比重瓶质量W3的测试:3. Test of the quality W 3 of the pycnometer filled with fiber and water:
(6)、将干燥后称过质量的纤维全部放入到比重瓶中,加满蒸馏水,将比重瓶放入盛有蒸馏水的烧杯中,并使水面没过比重瓶瓶口0.5mm,使比重瓶类似于“潜水艇”一样浸没于水中,将其一起放入抽真空装置中,控制真空度达到99.7%,保持12小时,然后将比重瓶放入密封罐中,使其温度稳定至室温20℃;(6), put all the fibers weighed after drying into the pycnometer, fill up with distilled water, put the pycnometer into a beaker filled with distilled water, and make the water surface 0.5mm over the mouth of the pycnometer, so that the specific gravity The bottle is immersed in water like a "submarine", put them together in a vacuum device, control the vacuum to 99.7%, keep it for 12 hours, and then put the pycnometer into a sealed tank to stabilize the temperature to room temperature 20 ℃;
(7)、称取装有纤维和水的比重瓶质量W3,利用阿基米德原理求出纤维的密度:(7), take by weighing the quality W 3 of the pycnometer that fiber and water are housed, utilize Archimedes principle to obtain the density of fiber:
上述的纤维比重的测试方法,其特征是:所述步骤(1)中烧杯中的蒸馏水没过比重瓶0.5cm。The above-mentioned test method of fiber specific gravity is characterized in that: the distilled water in the beaker in the step (1) has not passed the pycnometer for 0.5cm.
上述的纤维比重的测试方法,其特征是:所述步骤2中真空度设置为99.8%,保持2小时。The above-mentioned test method of fiber specific gravity is characterized in that: in the step 2, the vacuum degree is set to 99.8% and kept for 2 hours.
上述的纤维比重的测试方法,其特征是:所述步骤(4)中用无水酒精或乙醚浸泡纤维时间为35min,烘干温度为80℃,烘干时间为2h。The above-mentioned method for testing fiber specific gravity is characterized in that: in the step (4), the fiber is soaked in absolute alcohol or ether for 35 minutes, the drying temperature is 80° C., and the drying time is 2 hours.
本发明纤维比重的测试方法的优点是:本发明运用比重瓶法测定纤维的密度,具有操作简单,测试效率高,测试精度高的特点,可用于大量快速的测定各种纤维密度的测定。以往抽真空过程中比重瓶的水会不断的溢出,需要不断地往比重瓶中加水,新加入的水又会因产生气泡而部分溢出,即便不断加水,也很难以精确测定纤维的比重。本发明则直接将比重瓶放入一个盛有蒸馏水的烧杯中,并且保持烧杯中的蒸馏水没过比重瓶0.1~1cm左右,然后将烧杯连同比重瓶放入抽真空装置中抽真空,由于抽真空作用气泡会不断溢出,由于烧杯中的蒸馏水没过比重瓶,因此在气泡不断溢出的同时水会不断补入。抽真空过程要保持真空度达到99.5%以上,且不低于0.5小时,真空度越高越好,时间越长越好。最后,卸负压将比重瓶取出,放入密封罐中,至于20℃条件下平衡24小时后称其质量,计算纤维的比重。The advantage of the test method of fiber specific gravity of the present invention is: the present invention uses pycnometer method to measure the density of fiber, has the characteristics of simple operation, high test efficiency, high test precision, can be used for the mensuration of a large number of rapid determination of various fiber densities. In the past, the water in the pycnometer bottle would continuously overflow during the vacuuming process, and it was necessary to continuously add water to the pycnometer bottle, and the newly added water would partially overflow due to the generation of air bubbles. Even if the water was continuously added, it was difficult to accurately measure the specific gravity of the fiber. The present invention directly puts the pycnometer into a beaker filled with distilled water, and keeps the distilled water in the beaker submerged by about 0.1-1cm of the pycnometer, then puts the beaker together with the pycnometer into a vacuuming device to evacuate. The effect bubbles will continuously overflow, because the distilled water in the beaker has not passed the pycnometer, so water will continue to replenish when the bubbles continue to overflow. During the vacuuming process, the vacuum degree should be kept above 99.5%, and not less than 0.5 hours. The higher the vacuum degree, the better, and the longer the time, the better. Finally, remove the negative pressure and take out the pycnometer, put it into a sealed tank, balance it at 20°C for 24 hours, weigh it, and calculate the specific gravity of the fiber.
具体实施方式Detailed ways
下面结合具体实施例对本发明做进一步详细说明;Below in conjunction with specific embodiment the present invention is described in further detail;
实施例1:Example 1:
一种纤维比重的测试方法,包括如下步骤:A method for testing fiber specific gravity, comprising the steps:
一、仅装有水的比重瓶质量W1的测量:1. Measurement of the mass W 1 of a pycnometer filled with water only:
(1)、将灌满蒸馏水的100ml比重瓶放入盛有蒸馏水的150ml烧杯中,并且保持烧杯中的蒸馏水没过比重瓶0.1cm;(1), put the 100ml pycnometer filled with distilled water into the 150ml beaker filled with distilled water, and keep the distilled water in the beaker covered by 0.1cm of the pycnometer;
(2)、然后将烧杯连同比重瓶放入抽真空装置中抽真空,控制真空度达到99.5%,并保持3h:(2), then put the beaker together with the pycnometer into the vacuum device to evacuate, control the vacuum to 99.5%, and keep it for 3h:
(3)然后将比重瓶取出放入密封罐中至于20℃条件下平衡24h后称其质量,即得比重瓶+水的质量W1;(3) then take out the pycnometer and put it in a sealed tank, balance it for 24h under the condition of 20°C and weigh its quality, then get the quality W of the pycnometer+water;
二、纤维质量W2的测量:2. Measurement of fiber quality W 2 :
(4)、取待测定纤维20g,用无水酒精或乙醚浸泡纤维20min,去除纤维表面的油剂,然后在120℃环境中烘干时间在1h;(4) Take 20g of the fiber to be measured, soak the fiber with absolute alcohol or ether for 20min, remove the oil on the surface of the fiber, and then dry it at 120°C for 1h;
(5)、干燥完毕后用电子天平称量纤维的质量,标记为W2;(5), after drying, weigh the quality of fiber with electronic balance, marked as W 2 ;
三、装有纤维和水的比重瓶质量W3的测试:3. Test of the quality W 3 of the pycnometer filled with fiber and water:
(6)、将干燥后称过质量的纤维全部放入到比重瓶中,加满蒸馏水,将比重瓶放入盛有蒸馏水的烧杯中,并使水面没过比重瓶瓶口0.5mm,使比重瓶类似于“潜水艇”一样浸没于水中,将其一起放入抽真空装置中,控制真空度达到99.7%,保持12小时,然后将比重瓶放入密封罐中,使其温度稳定至室温20℃;(6), put all the fibers weighed after drying into the pycnometer, fill up with distilled water, put the pycnometer into a beaker filled with distilled water, and make the water surface 0.5mm over the mouth of the pycnometer, so that the specific gravity The bottle is immersed in water like a "submarine", put them together in a vacuum device, control the vacuum to 99.7%, keep it for 12 hours, and then put the pycnometer into a sealed tank to stabilize the temperature to room temperature 20 ℃;
(7)、称取装有纤维和水的比重瓶质量W3,利用阿基米德原理求出纤维的密度:(7), take by weighing the quality W 3 of the pycnometer that fiber and water are housed, utilize Archimedes principle to obtain the density of fiber:
尽管纤维在水中会不同程度的因吸湿而膨胀,但是由于该方法中的脱泡和补水是一个连续的过程显著地减少了气泡对实验结果的影响,具有精度高、重现性好、稳定性好的优点,即使测试棉纤维的比重,其结果也基本稳定在1.535~1.550之间,与国内外公认的数据相一致。当然用该方法测试吸湿较小的丙纶、涤纶、腈纶、锦纶等纤维比重则更快,3小时即可;数据更稳定,均差在0.003左右。Although the fiber will swell to varying degrees due to moisture absorption in water, since the defoaming and water replenishment in this method are a continuous process, the influence of air bubbles on the experimental results is significantly reduced, and it has high precision, good reproducibility and stability. Good advantage, even if the specific gravity of cotton fiber is tested, the result is basically stable between 1.535 and 1.550, which is consistent with the recognized data at home and abroad. Of course, using this method to test the specific gravity of polypropylene, polyester, acrylic, nylon and other fibers with less hygroscopicity is faster, within 3 hours; the data is more stable, with an average difference of about 0.003.
实施例2:Example 2:
一种纤维比重的测试方法,包括如下步骤:A method for testing fiber specific gravity, comprising the steps:
一、仅装有水的比重瓶质量W1的测量:1. Measurement of the mass W 1 of a pycnometer filled with water only:
(1)、将灌满蒸馏水的100ml比重瓶放入盛有蒸馏水的150ml烧杯中,并且保持烧杯中的蒸馏水没过比重瓶0.5cm;(1), put the 100ml pycnometer filled with distilled water into a 150ml beaker filled with distilled water, and keep the distilled water in the beaker covered by 0.5cm of the pycnometer;
(2)、然后将烧杯连同比重瓶放入抽真空装置中抽真空,控制真空度达到99.8%,并保持2h;(2), then put the beaker together with the pycnometer into a vacuum device to evacuate, control the vacuum degree to 99.8%, and keep it for 2h;
(3)然后将比重瓶取出放入密封罐中至于20℃条件下平衡24h后称其质量,即得比重瓶+水的质量W1;(3) then take out the pycnometer and put it in a sealed tank, balance it for 24h under the condition of 20°C and weigh its quality, then get the quality W of the pycnometer+water;
二、纤维质量W2的测量:2. Measurement of fiber quality W 2 :
(4)、取待测定纤维20g,用无水酒精或乙醚浸泡纤维35min,去除纤维表面的油剂,然后在80℃环境中烘干时间在2h;(4) Take 20g of the fiber to be measured, soak the fiber with absolute alcohol or ether for 35 minutes, remove the oil on the surface of the fiber, and then dry it at 80°C for 2 hours;
(5)、干燥完毕后用电子天平称量纤维的质量,标记为W2;(5), after drying, weigh the quality of fiber with electronic balance, marked as W 2 ;
三、装有纤维和水的比重瓶质量W3的测试:3. Test of the quality W 3 of the pycnometer filled with fiber and water:
(6)、将干燥后称过质量的纤维全部放入到比重瓶中,加满蒸馏水,将比重瓶放入盛有蒸馏水的烧杯中,并使水面没过比重瓶瓶口0.5mm,使比重瓶类似于“潜水艇”一样浸没于水中,将其一起放入抽真空装置中,控制真空度达到99.7%,保持12小时,然后将比重瓶放入密封罐中,使其温度稳定至室温20℃;(6), put all the fibers weighed after drying into the pycnometer, fill up with distilled water, put the pycnometer into a beaker filled with distilled water, and make the water surface 0.5mm over the mouth of the pycnometer, so that the specific gravity The bottle is immersed in water like a "submarine", put them together in a vacuum device, control the vacuum to 99.7%, keep it for 12 hours, and then put the pycnometer into a sealed tank to stabilize the temperature to room temperature 20 ℃;
(7)、称取装有纤维和水的比重瓶质量W3,利用阿基米德原理求出纤维的密度:(7), take by weighing the quality W 3 of the pycnometer that fiber and water are housed, utilize Archimedes principle to obtain the density of fiber:
实施例3:Example 3:
一种纤维比重的测试方法,包括如下步骤:A method for testing fiber specific gravity, comprising the steps:
一、仅装有水的比重瓶质量W1的测量:1. Measurement of the mass W 1 of a pycnometer filled with water only:
(1)、将灌满蒸馏水的100ml比重瓶放入盛有蒸馏水的150ml烧杯中,并且保持烧杯中的蒸馏水没过比重瓶0.1cm;(1), put the 100ml pycnometer filled with distilled water into the 150ml beaker filled with distilled water, and keep the distilled water in the beaker covered by 0.1cm of the pycnometer;
(2)、然后将烧杯连同比重瓶放入抽真空装置中抽真空,控制真空度达到99.9%,并保持1h:(2), then put the beaker together with the pycnometer into a vacuum device to evacuate, control the vacuum to 99.9%, and keep it for 1h:
(3)然后将比重瓶取出放入密封罐中至于20℃条件下平衡24h后称其质量,即得比重瓶+水的质量W1;(3) then take out the pycnometer and put it in a sealed tank, balance it for 24h under the condition of 20°C and weigh its quality, then get the quality W of the pycnometer+water;
二、纤维质量W2的测量:2. Measurement of fiber quality W 2 :
(4)、取待测定纤维20g,用无水酒精或乙醚浸泡纤维50min,去除纤维表面的油剂,然后在50℃环境中烘干时间在3h;(4) Take 20g of the fiber to be measured, soak the fiber with absolute alcohol or ether for 50min, remove the oil on the surface of the fiber, and then dry it at 50°C for 3h;
(5)、干燥完毕后用电子天平称量纤维的质量,标记为W2;(5), after drying, weigh the quality of fiber with electronic balance, marked as W 2 ;
三、装有纤维和水的比重瓶质量W3的测试:3. Test of the quality W 3 of the pycnometer filled with fiber and water:
(6)、将干燥后称过质量的纤维全部放入到比重瓶中,加满蒸馏水,将比重瓶放入盛有蒸馏水的烧杯中,并使水面没过比重瓶瓶口0.5mm,使比重瓶类似于“潜水艇”一样浸没于水中,将其一起放入抽真空装置中,控制真空度达到99.7%,保持12小时,然后将比重瓶放入密封罐中,使其温度稳定至室温20℃;(6), put all the fibers weighed after drying into the pycnometer, fill up with distilled water, put the pycnometer into a beaker filled with distilled water, and make the water surface 0.5mm over the mouth of the pycnometer, so that the specific gravity The bottle is immersed in water like a "submarine", put them together in a vacuum device, control the vacuum to 99.7%, keep it for 12 hours, and then put the pycnometer into a sealed tank to stabilize the temperature to room temperature 20 ℃;
(7)、称取装有纤维和水的比重瓶质量W3,利用阿基米德原理求出纤维的密度:(7), take by weighing the quality W 3 of the pycnometer that fiber and water are housed, utilize Archimedes principle to obtain the density of fiber:
当然,上述说明并非是对本发明的限制,本发明也并不限于上述举例,本技术领域的普通技术人员,在本发明的实质范围内,作出的变化、改型、添加或替换,都应属于本发明的保护范围。Of course, the above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Any changes, modifications, additions or substitutions made by those skilled in the art within the scope of the present invention shall all belong to protection scope of the present invention.
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CN107290252A (en) * | 2017-06-30 | 2017-10-24 | 浙江石金玄武岩纤维股份有限公司 | A kind of method for testing fiber wetness energy |
CN107290252B (en) * | 2017-06-30 | 2019-10-11 | 浙江石金玄武岩纤维股份有限公司 | A method of test fiber wetness can |
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CN109916770A (en) * | 2019-03-15 | 2019-06-21 | 同济大学 | A method for determining the density of polymer particles |
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