CN104062285A - Determination method for contents of calcium, aluminum and silicon elements in solid surface materials - Google Patents
Determination method for contents of calcium, aluminum and silicon elements in solid surface materials Download PDFInfo
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- CN104062285A CN104062285A CN201410333606.7A CN201410333606A CN104062285A CN 104062285 A CN104062285 A CN 104062285A CN 201410333606 A CN201410333606 A CN 201410333606A CN 104062285 A CN104062285 A CN 104062285A
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Abstract
The invention discloses a determination method for contents of calcium, aluminum and silicon elements in solid surface materials. After the solid surface materials are treated by adopting a sodium hydroxide alkali fusion method, a standard addition method is used for determining the contents of the calcium, aluminum and silicon elements in the solid surface materials. The sodium hydroxide alkali fusion method is adopted to realize the treatment on solid surface material samples; an ICP-OES (Inductively Coupled Plasma-Optical Emission Spectroscopy) technology is used for performing accurate determination of the contents of filler components of the solid surface materials; the research result is used for establishing a chemical component detection method for the solid surface materials. Compared with the prior art, the accurate detection on the varieties and the contents of current solid surface material filler is realized; the standard addition method is applied so that the accuracy of testing the contents of the filler components of the solid surface materials is improved.
Description
Technical field
The invention belongs to entity plane materiel technical field, particularly the assay method of calcium, aluminium, silicon content in a kind of entity plane materiel.
Background technology
The filler part of artificial stone mainly contains silicon dioxide, aluminium hydroxide and calcium carbonate three types.The contamination of packing material plays a very important role aspect properties of product, for example filler is the entity plane materiel of natural stone material (principal ingredient is calcium carbonate), the mechanical properties such as its compression, bending are well below quartz, simultaneously there is radioactivity and glossiness is poor etc. that shortcoming also attracts much attention gradually in natural stone material, but because the raw materials cost of this series products is lower, price competitiveness is relatively high, and some illegal manufacturing enterprises substitute the bad for the good successively and cheat consumer.In view of development course and the experience and lessons of home market entity plane materiel, and the method for Accurate Determining entity plane materiel filling kind and content lacks very much, (fourth is for army building for fourth grade for army building, Mei Yifei, Hu Yunlin. entity plane materiel aluminium hydroxide, the mensuration of calcium carbonate and resin content. stone material. 2013, 12, 35-37.) adopt thermogravimetric analysis to be studied entity plane materiel media assemblage and content, but the method can not be measured kind and the content of filler very accurately, and also very limited to the detection of filling kind, therefore the research of carrying out entity plane materiel filling kind and content accurate detecting method is very necessary.
Summary of the invention
Goal of the invention: for the problem and shortage of above-mentioned prior art existence, the object of this invention is to provide the assay method of calcium, aluminium, silicon content in a kind of entity plane materiel.
Technical scheme: in order to solve the problems of the technologies described above, technical scheme provided by the invention is as follows: the assay method of calcium, aluminium, silicon content in a kind of entity plane materiel, entity plane materiel is processed to rear employing standard addition method by the method for sodium hydroxide alkali fusion calcium, aluminium, silicon content in entity plane materiel are measured, concrete steps are as follows:
1) take entity plane materiel sample 0.5 ~ 1g, add the NaOH solid of 5～6 g to be placed in silver crucible, first in 350 DEG C of muffle furnaces, react 2h, then temperature is risen to 600 DEG C and continue reaction 30 min, cooling, silver crucible is put into the beaker heating that contains 100mL water to be boiled and adds wherein 25～30mL hydrochloric acid, treat that sample dissolves taking-up silver crucible completely and rinses, in solution, add 1 mL red fuming nitric acid (RFNA), continue to boil in 1 min, cooling 250 mL that are settled to obtain testing sample, prepare parallel blank sample by above-mentioned identical experimental procedure, finally be settled to 250 mL and obtain blank solution,
2) prepare respectively the mixed standard solution that contains calcium, aluminium, element silicon of 2ppm, 4ppm, 6ppm, 8ppm, and drawing standard curve;
3) pipette the blank solution in 1 mL step 1), be diluted to 100 mL as blank standard specimen, pipetting respectively testing sample in 1 mL step 1) puts into 5 100 mL volumetric flasks and is designated as S1, S2, S3, S4, S5, in S2, S3, S4, S5, add concentration to be followed successively by the mixed standard solution that contains calcium, aluminium, element silicon of 2ppm, 4ppm, 6ppm, 8ppm, be settled to 100 mL, treat ICP-OES analytical test.
Wherein, described step 2) in contain calcium, aluminium, element silicon mixed standard solution compound method as follows: the CaCO that takes respectively 75.3734 g, 75.2783 g, 75.2169 g
3, Al (OH)
3and SiO
2mix and fully mix, three parts of weight such as being divided into, a copy of it weight is 75.3651 g, adds wherein the adjacent benzene type unsaturated polyester (L) of 25.0643 g; A weight is 75.2108 g, adds wherein the metaphenylene unsaturated polyester (J) of 25.3128 g; A weight is 75.2310 g, add wherein the polymethylmethacrylate (Y) of 25.5102 g, after fully stirring and evenly mixing, in above-mentioned three parts of samples, add respectively 0.08 g hardening agent cobalt iso-octoate and 0.30 g promoter methyl ethyl ketone peroxide and fully stir, under 60 DEG C of conditions, making it solidify and obtain target product S
l, S
j, S
y.
Beneficial effect: compared with prior art, this method has realized the processing of entity plane materiel sample by the method for sodium hydroxide alkali fusion, utilize ICP-OES technology to obtain the Accurate Measurement to entity plane materiel filler component content, this achievement in research has been established entity plane materiel chemical composition detection method.The application has solved the accurate detection of current entity face material stuffing kind and content with respect to prior art, by using standard addition method, improved the accuracy of entity plane materiel filer content test.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.
Embodiment 1:
Take 0.5 g entity plane materiel sample, be accurate to 0.0001 g, add the NaOH solid of 5～6 g to be placed in silver crucible, first in 350 DEG C of muffle furnaces, react 2 h, then temperature is risen to 600 DEG C and continue reaction 30 min, cooling.Silver crucible is put into the beaker heating that contains 100 mL water and boil and add wherein 25～30 mL hydrochloric acid, treat that sample dissolves taking-up silver crucible completely and rinses, in solution, add 1 mL red fuming nitric acid (RFNA), continue to boil in 1 min cooling 250 mL that are settled to.Prepare parallel blank sample by above-mentioned identical experimental procedure, be finally settled to 250 mL.1) standard addition method
Pipette the above-mentioned blank solution of 1 mL, be diluted to 100 mL as blank standard specimen, the testing sample that pipettes 1 mL is put into respectively 5 100 mL volumetric flasks and is designated as S1, S2, S3, S4, S5, according to the concentration of experimental design Si, Al, Ca be followed successively by 2 ppm, 4 ppm, 6 ppm, 8 ppm add Si, Al, Ca standard solution to S2, S3, S4, S5, be settled to 100 mL, the concentration of Si, Al, Ca is followed successively by 2 ppm, 4 ppm, 6 ppm, 8 ppm, treats ICP-OES analytical test.
Prepare Si, Al, the Ca mixed standard solution of 2 ppm, 4 ppm, 6 ppm, 8 ppm, and drawing standard curve, in order to calculate the concentration of Si in sample to be tested, Al, Ca ion.
Embodiment 2
The sample media assemblage test of the identical media assemblage of different matrix.
The preparation of sample is with reference to the test method of Xing Bangyuan etc., and concrete experimental detail has part to change.CaCO3, Al (OH) 3 and the SiO2 that take respectively 75.3734 g, 75.2783 g, 75.2169 g mix and fully mix, three parts of weight such as be divided into, a copy of it weight is 75.3651g, adds wherein the adjacent benzene type unsaturated polyester (L) of 25.0643g; A weight is 75.2108g, adds wherein the metaphenylene unsaturated polyester (J) of 25.3128g; A weight is 75.2310g, add wherein the polymethylmethacrylate (Y) of 25.5102g, after fully stirring and evenly mixing, in above-mentioned three parts of samples, add respectively 0.08 g hardening agent cobalt iso-octoate and 0.30 g promoter methyl ethyl ketone peroxide and fully stir, under 60 DEG C of conditions, make it solidify and obtain target product, difference called after SL, SJ, SY successively.
Two kinds of SiO2, Al (OH) 3 and high samples of CaCO3 content that method of testing forms different matrix, result and actual value gap that these two kinds of method of testings obtain are not obvious, and measured value and the actual value of standard addition method are more approaching.
Embodiment 3
The sample media assemblage test of the different media assemblages of same matrix.
After Al (OH) 3, CaCO3, the SiO2 that weighs successively 69.2267 g, 2.0070 g, 3.1663 g fully mixes, add the polymethylmethacrylate of 25.8637 g fully to stir and evenly mix.After Al (OH) 3, SiO2, CaCO3, the SiO2 that weighs successively 2.1394 g, 70.9048 g, 1.6557 g fully mixes, add the polymethylmethacrylate of 25.0136 g fully to stir and evenly mix; After Al (OH) 3, SiO2, the CaCO3 sample that takes successively 2.2682 g, 3.1152 g, 68.2166 g fully mixes, add the polymethylmethacrylate of 25.0321 g fully to stir and evenly mix, in the sample of above-mentioned three kinds of different compositions, respectively add respectively 0.08 g hardening agent cobalt iso-octoate and 0.30 g promoter methyl ethyl ketone peroxide fully to stir and evenly mix, under 60 DEG C of conditions, make it solidify and obtain target product, difference called after S-Al, S-Ca, S-Si successively.
But for the sample of the different media assemblages of same matrix, especially SiO2, Al (OH) 3 and the low sample of CaCO3 content, the object percentage composition that standard addition method is measured obviously more approaches actual weighing value than calibration curve method measurement target thing percentage composition, and this phenomenon all shows the more close actual weighing value of measured value of standard addition method in the sample of different media assemblages.Therefore, we are more suitable for the detection of filler composition in the entity plane materiel of NaOH high temperature alkali fuse at the standard addition method of reaching a conclusion, and measurement result is more accurate than calibration curve method.
Claims (2)
1. the assay method of calcium, aluminium, silicon content in an entity plane materiel, it is characterized in that, entity plane materiel is processed to rear employing standard addition method by the method for sodium hydroxide alkali fusion calcium, aluminium, silicon content in entity plane materiel are measured, concrete steps are as follows:
1) take entity plane materiel sample 0.5 ~ 1g, add the NaOH solid of 5～6 g to be placed in silver crucible, first in 350 DEG C of muffle furnaces, react 2h, then temperature is risen to 600 DEG C and continue reaction 30 min, cooling, silver crucible is put into the beaker heating that contains 100mL water to be boiled and adds wherein 25～30mL hydrochloric acid, treat that sample dissolves taking-up silver crucible completely and rinses, in solution, add 1 mL red fuming nitric acid (RFNA), continue to boil in 1 min, cooling 250 mL that are settled to obtain testing sample, prepare parallel blank sample by above-mentioned identical experimental procedure, finally be settled to 250 mL and obtain blank solution,
2) prepare respectively the mixed standard solution that contains calcium, aluminium, element silicon of 2ppm, 4ppm, 6ppm, 8ppm, and drawing standard curve;
3) pipette the blank solution in 1 mL step 1), be diluted to 100 mL as blank standard specimen, pipetting respectively testing sample in 1 mL step 1) puts into 5 100 mL volumetric flasks and is designated as S1, S2, S3, S4, S5, in S2, S3, S4, S5, add concentration to be followed successively by the mixed standard solution that contains calcium, aluminium, element silicon of 2ppm, 4ppm, 6ppm, 8ppm, be settled to 100 mL, treat ICP-OES analytical test.
2. the assay method of calcium, aluminium, silicon content in a kind of entity plane materiel according to claim 1, it is characterized in that described step 2) in contain calcium, aluminium, element silicon mixed standard solution compound method as follows: the CaCO that takes respectively 75.3734 g, 75.2783 g, 75.2169 g
3, Al (OH)
3and SiO
2mix and fully mix, three parts of weight such as being divided into, a copy of it weight is 75.3651g, adds wherein the adjacent benzene type unsaturated polyester of 25.0643g; A weight is 75.2108 g, adds wherein the metaphenylene unsaturated polyester of 25.3128 g; A weight is 75.2310 g, add wherein the polymethylmethacrylate of 25.5102 g, after fully stirring and evenly mixing, in above-mentioned three parts of samples, add respectively 0.08 g hardening agent cobalt iso-octoate and 0.30 g promoter methyl ethyl ketone peroxide and fully stir, under 60 DEG C of conditions, making it solidify and obtain respectively target product S
l, S
j, S
y.
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| CN104730098A (en) * | 2015-04-03 | 2015-06-24 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Rapid analysis method of high-content harmful element in blast furnace iron material |
| CN109884036A (en) * | 2019-03-08 | 2019-06-14 | 国家硅材料深加工产品质量监督检验中心东海研究院 | A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104713871A (en) * | 2015-02-09 | 2015-06-17 | 南京市产品质量监督检验院 | Detection method of heavy metals Pb, Cd, Cr and Hg in solid surfacing material |
| CN104730098A (en) * | 2015-04-03 | 2015-06-24 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Rapid analysis method of high-content harmful element in blast furnace iron material |
| CN109884036A (en) * | 2019-03-08 | 2019-06-14 | 国家硅材料深加工产品质量监督检验中心东海研究院 | A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz |
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| CN104062285B (en) | 2017-09-19 |
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Effective date of registration: 20190828 Address after: 210000 Nanjing Quality and Safety Technology Center, No. 3 East Street, Jialing River, Nanjing City, Jiangsu Province Co-patentee after: Shenzhen city Ning inspection and Testing Technology Co., Ltd. Patentee after: Nanjing Product Quality Supervision and Inspection Institute Address before: 210000 Hongshan Road, Xuanwu District, Jiangsu, Nanjing 168 Patentee before: Nanjing Product Quality Supervision and Inspection Institute |
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