CN112326705A

CN112326705A - Qualitative identification method of basalt fibers

Info

Publication number: CN112326705A
Application number: CN202011367536.9A
Authority: CN
Inventors: 马辉; 朱锦波; 石岩; 姚传刚
Original assignee: Tianjin Customs Metal Material Testing Center
Current assignee: Tianjin Customs Metal Material Testing Center
Priority date: 2020-11-30
Filing date: 2020-11-30
Publication date: 2021-02-05
Anticipated expiration: 2040-11-30
Also published as: CN112326705B

Abstract

The invention relates to a qualitative identification method of basalt fibers, which comprises the following steps of (1) analyzing by using an X-ray diffractometer, wherein the diffraction result is amorphous; (2) placing a fiber sample to be detected in a ceramic crucible, placing the ceramic crucible and the fiber sample into a muffle furnace at the temperature of 850-950 ℃, preserving heat for 4-6 hours until the sample becomes brittle and grindable particles, and grinding the sample into fine powder with the particle size of 100-200 meshes by hand or machine after cooling; (3) respectively putting the fine powder sample into an X-ray fluorescence spectrometer and an X-ray diffraction analyzer for analysis, and measuring SiO in the sample by the X-ray fluorescence spectrometer₂The content is 30% -60%, the phase of the X-ray diffraction analysis sample is one or more minerals with crystal form, and can display obvious diffraction characteristic peak; (4) and (4) according to the test results of the steps (1) and (3), qualitatively identifying the sample as the basalt fiber. The operation is simple, convenient and safe, the result is accurate and visual, the operation requirement on testing personnel is not high, and various tests are not required to be mutually adjuvanted.

Description

Qualitative identification method of basalt fibers

Technical Field

The invention relates to an identification method of mineral fibers, in particular to a qualitative identification method of basalt fibers.

Background

The basalt fiber is a continuous fiber which is prepared by using various basalt, diabase and other similar rocks as raw materials, melting at a high temperature of 1450-1500 ℃, and then carrying out a wire drawing preparation process, and is collectively called as the basalt fiber. The basalt fiber-containing products mainly comprise basalt fiber powder, basalt fiber boards, basalt fiber filaments or yarns, various basalt fiber woven products such as basalt fiber cloth, felt and related products thereof, rock wool boards and the like.

The existing basalt fiber qualitative identification standard is SN/T4357-2015 ceramic, basalt, polyphenylene sulfide and polyether ether ketone fiber qualitative analysis for import and export textile fiber, and the basalt fiber qualitative identification method is specified. The qualitative identification method mainly refers to a common identification method in serial standards of FZ/T01057-2007 textile fiber identification test method, and tests the combustion characteristics, appearance form, solubility, initial thermal decomposition temperature and density of the basalt fiber respectively, and comprehensively identifies the basalt fiber according to the test result.

The comprehensive identification principle of the standard SN/T4357-2015 for the basalt fibers is finally determined after identification by a combustion test method and further confirmation by one or more methods such as a chemical dissolution method, a thermal analysis method and a density method. The identification process requires that the individual tests be mutually adjuvanted. The chemical dissolution test needs strong acid, strong base and toxic reagent, the microscopy, the thermal analysis and the density method need special instruments and equipment, the test process has high requirements on testers, and the whole identification process is complicated.

Disclosure of Invention

In view of the problems in the prior art, the invention provides a method for qualitatively identifying basalt fibers, which can be used for qualitatively identifying basalt fibers only by directly testing through an X-ray fluorescence spectrometer and an X-ray diffraction analyzer after heating and heat preservation treatment at a certain temperature is carried out on a sample without adopting various test methods for comprehensive identification. The specific technical scheme is that the method for qualitatively identifying the basalt fibers is characterized by comprising the following steps: the qualitative identification method comprises (1) making the fiber product to be detected into the shape and size of the sample required by the diffractometer, and analyzing with X-ray diffractometer to obtain amorphous diffraction result; (2) 50g to 200g of a fiber sample to be detected is placed in a ceramic crucible and put into a muffle furnace with the temperature of 850 ℃ to 950 DEG CKeeping the temperature for 4-6 h, wherein the heat preservation time can be discontinuous and can be interrupted in the midway until the sample is changed into brittle and grindable crushed particles, and grinding the sample into fine powder with the granularity of 100-200 meshes by hand or a machine after cooling; (3) respectively putting the prepared fine powder sample into an X-ray fluorescence spectrometer and an X-ray diffraction analyzer for analysis, and measuring SiO in the sample by the X-ray fluorescence spectrometer₂The content is 30-60%, the phase of the X-ray diffraction analysis sample is one or more minerals with crystal morphology, such as pyroxene, feldspar, olivine, leucite and quartz, and can display obvious diffraction characteristic peaks; (4) and (4) according to the test results of the steps (1) and (3), qualitatively identifying the sample as the basalt fiber.

The method has the advantages of simple, convenient, accurate and visual operation steps, no need of mutual evidence of various test methods, no need of using strong acid, strong base and toxic reagents, and low operation requirement of test personnel in the test process.

Drawings

FIG. 1 is a graph of the diffraction results of an original sample of the present invention;

FIG. 2 is a graph showing diffraction results of a sample of the present invention after heat-holding treatment.

Detailed Description

The present invention will be further described with reference to the following examples and accompanying drawings.

As shown in fig. 1 and fig. 2, the qualitative identification method comprises the steps of,

(1) taking a proper amount of rock wool, preparing a sample required by a diffractometer, and analyzing by using an X-ray diffractometer, wherein the diffraction result is amorphous;

(2) placing at least 50g of rock wool sample in a ceramic crucible, placing the ceramic crucible and the rock wool sample in a muffle furnace at 950 ℃, preserving heat for at least 4h, heating and preserving heat intermittently in the process until the sample becomes brittle and grindable crushed particles, and manually grinding the sample into fine powder with the particle size of 200 meshes after cooling;

(3) respectively putting the fine powder sample into an X-ray fluorescence spectrometer and an X-ray diffraction analyzer for analysis, and measuring SiO in the sample by the X-ray fluorescence spectrometer₂The content is within 30-60 percent, the sample phase is pyroxene after X-ray diffraction analysis, and the pyroxene is obviousShowing distinct diffraction characteristic peaks;

(4) and (4) according to the test results of the steps (1) and (3), the sample can be qualitatively identified as the basalt fiber.

Claims

1. A qualitative identification method of basalt fibers is characterized by comprising the following steps: the qualitative identification method comprises the following steps of,

(1) taking a measured fiber product to prepare the shape and the size of a sample required by an X-ray diffractometer, and analyzing by using the X-ray diffractometer, wherein the diffraction result is amorphous;

(2) placing 50 g-200 g of a fiber sample to be detected in a ceramic crucible, placing the ceramic crucible and the fiber sample into a muffle furnace at the temperature of 850-950 ℃, preserving heat for 4-6 h, wherein the heat preservation time can be discontinuous and can be discontinuous in the midway until the sample becomes brittle and grindable crushed particles, and grinding the sample into fine powder with the particle size of 100-200 meshes manually or by a machine after cooling;

(3) respectively putting the prepared fine powder sample into an X-ray fluorescence spectrometer and an X-ray diffraction analyzer for analysis, and measuring SiO in the sample by the X-ray fluorescence spectrometer₂The content is 30-60%, the phase of the X-ray diffraction analysis sample is one or more minerals with crystal morphology, such as pyroxene, feldspar, olivine, leucite and quartz, and can display obvious diffraction characteristic peaks;

(4) and (4) according to the test results of the steps (1) and (3), qualitatively identifying the sample as the basalt fiber.