CN104316431A - Method for detecting content of diatomaceous earth in diatom ooze wall material - Google Patents
Method for detecting content of diatomaceous earth in diatom ooze wall material Download PDFInfo
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- CN104316431A CN104316431A CN201410625223.7A CN201410625223A CN104316431A CN 104316431 A CN104316431 A CN 104316431A CN 201410625223 A CN201410625223 A CN 201410625223A CN 104316431 A CN104316431 A CN 104316431A
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Abstract
The invention provides a method for detecting the content of diatomaceous earth in a diatom ooze wall material. The method adopts step heat treatment, water, organic components and volatile component in a sample are removed, then silicate in the sample is dissolved at a certain temperature by using pyrophosphoric acid, and SiO2 to be detected remains after washing, so that the content of the diatomaceous earth is detected more accurately, truly and reliably. According to the method provided by the invention, operating steps are simplified, used equipment is low in cost and easy to obtain, and the method is scientific, reasonable and high in operability. Through comparison with a sample with known content, the recovery rate is high, and the result is satisfactory.
Description
Technical field
The present invention relates to the assay method of zeyssatite content in diatom ooze wall material, belong to the mensuration field of material composition content.
Background technology
Zeyssatite is a kind of biogenic silicastone, and principal ingredient is SiO
2, have that light porous, specific surface area is large, chemical stability high, its particle surface is with electric charge usually, and absorption property is good.Therefore have and purify air, breathe damping, repel the function that dust, antibacterial and deodouring, fire protection flame retarding, sound-absorbing noise abatement etc. improve living environment.Improving constantly and requiring more and more higher to living environment along with people's living standard, with the addition of diatomaceous diatom ooze wall material and is progressively commonly used by people for indoor wall ornament materials.Diatom ooze becomes to be grouped into primarily of zeyssatite, basic powder, adjuvant, aggregate etc., chemically material property is exactly by SiO
2, the silicate of various metal and organism composition.Current diatom ooze wall material market is numerous confused complexity, very different, and competition is also abnormal fierce, is mainly manifested in three aspects: unprofessional, unstable, lack of standardization.What is more utilizes not understanding of client, diatom ooze is pretended to be with other materials (white cement, gypsum, powder of lacquer putty for use on, gelling thing), bring potential hidden danger to diatom ooze industry, cause it to be " industry that China's fraud is the most mad " bad impression like this.
Although state to some extent the assay method of diatom composition in national sector standard " diatom ooze decorative wall material ", but the equipment price such as X-ray diffractometer, electron microscope that the method is used is high, operation is comparatively complicated, and the method cannot accomplish to carry out accurate quantitative analysis to diatom composition.What adopt the mensuration of zeyssatite content in industry standard " zeyssatite and test method thereof " is fluoric acid silicon potassium capacity method, but the method is in practical operation, the interference of silicate cannot be got rid of, also just cannot really accomplish to differentiate " true and false " of diatom ooze, and pre-treatment step is loaded down with trivial details, terminal difficulty judges, finally has influence on the accuracy of result.Therefore, develop more can accurately, the detection method of zeyssatite content in true working sample, to specification diatom ooze wall material market and to carry out effectively supervision to it significant.
Summary of the invention
Based on this, the object of the invention is to get rid of the interference of silicate, overcome chemical capacity method pre-treatment step loaded down with trivial details, the shortcoming that terminal difficulty judges, a kind of simple to operate, method that result detects zeyssatite content in diatom ooze wall material is accurately provided.
Adopt moisture, the organic and volatile ingredient in substep thermal treatment removing sample, then with the silicate in pyrophosphoric acid at a certain temperature sample dissolution, through washing, remaining is the SiO that will measure
2.The method progressively can remove non-targeted thing pointedly, clear thinking, simple to operate.
The technical solution used in the present invention is as follows:
An assay method for zeyssatite content in diatom ooze wall material, comprises the following steps:
Step 1: take appropriate amount of sample dry under uniform temperature, to remove moisture;
Step 2: take dry sample in crucible, calcination under high temperature, with organics removal and volatile ingredient;
Step 3: be stirred in electric hot plate top heating edge after adding pyrophosphoric acid in the sample after calcination and react completely, reactant liquor is slowly poured in beaker filled with hot water, with Filter paper filtering, with watery hydrochloric acid, residue precipitation in beaker is washed funnel completely again, reusable heat water rinses and is precipitated to neutrality, to remove silicate;
Step 4: crucible filter paper being put into constant weight, at high temperature calcination is to constant weight, obtains zeyssatite.
Preferably, the drying condition of sample is: dry 4h at 105 DEG C ± 2 DEG C.
Preferably, the calcination condition of dry sample is: calcination 1h at 850 DEG C ± 25 DEG C.
Preferably, the step removing silicate is: be stirred in 250 DEG C of electric hot plate top heating edge after adding 20mL pyrophosphoric acid in the sample after calcination and react completely; Slowly poured into by reactant liquor and filled in the 400mL beaker of 200mL hot water, filter while hot, with the watery hydrochloric acid of 0.1mol/L, residue precipitation in beaker is washed funnel completely, reusable heat water rinses and is precipitated to neutrality.
Preferably, after removing silicate, final acquisition object SiO
2step be: crucible filter paper being put into constant weight, at 850 DEG C ± 25 DEG C, calcination is to constant weight.
Wherein, SiO is calculated as follows
2content (%)
In formula: m-take dry rear sample mass, g;
M
0empty crucible quality after-pre-burn, g;
M
1crucible and precipitation quality after-pre-burn, g.
Compared with prior art, the present invention has the following advantages: the present invention is applicable to the mensuration of zeyssatite content in diatom ooze wall material, each step can remove non-targeted thing pointedly, the most important thing is the interference getting rid of silicate, the method methodological science is reasonable, workable, and there is the function differentiating diatom ooze " true and false ".
Embodiment
The present invention is described in further detail below, and all technology realized based on content of the present invention all belong to scope of the present invention.
1, instrument and equipment
Electronic balance (being accurate to 0.lmg), electric hot plate, muffle furnace
2, reagent is selected
Pyrophosphoric acid (chemical pure);
Watery hydrochloric acid (0.1mol/L): with measuring 4.2mL hydrochloric acid, pour in beaker along glass bar, then add a small amount of water (about 60mL), slowly stir with glass bar, make it mix; The hydrochloric acid cooled is injected the volumetric flask of 500mL along glass bar; With 30mL water washing beaker 2-3 time, the equal injection capacity bottle of cleansing solution, constant volume, shakes up.
3, operation steps
(1) moisture is removed: take appropriate amount of sample under preference temperature after drying, cooling.
(2) organics removal and volatile matter: take appropriate (being accurate to 0.1mg) dry sample in platinum crucible, calcination in high temperature furnace, cooling.
(3) silicate is removed: be stirred in electric hot plate top heating edge after adding 20mL pyrophosphoric acid and react completely.Slowly poured into by reactant liquor and filled in the 400mL beaker of 200mL hot water, filter while hot, with the watery hydrochloric acid of 0.1mol/L, residue precipitation in beaker is washed funnel completely, reusable heat water rinses and is precipitated to neutrality.
(4) object SiO is obtained
2: crucible filter paper being put into constant weight, in high temperature furnace, calcination is to constant weight.
4, result calculates:
Calculate SiO as follows
2content (%)
In formula: m-take dry rear sample mass, g;
M
0empty crucible quality after-pre-burn, g;
M
1crucible and precipitation quality after-pre-burn, g.
5, detection method evaluation
The composition of diatom ooze wall material is mainly zeyssatite, silica sand, porcelain earth, sepiolite.In order to verify the accuracy of this detection method, adopt following experimental verification:
(1) uniform verification sample is prepared according to following proportioning.
(2) blank sample is prepared.
(3) 0.2g 0 is taken respectively
#, 1
#, 2
#, 3
#dry sample, through calcination, pyrophosphoric acid process, washing, calcination, result is as follows:
As can be seen from the above table, measured value and the recovery are all satisfactory, and what prove that the present invention sets up is feasible for the assay method of zeyssatite content in diatom ooze.This process simplify operation steps, device therefor is cheap and easy to get, and methodological science is reasonable, workable.By contrasting with known content sample, the recovery is up to 98.1%, and result is satisfactory.
In addition, be to be understood that, although this instructions is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of instructions is only for clarity sake, those skilled in the art should by instructions integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (7)
1. the assay method of zeyssatite content in diatom ooze wall material, is characterized in that, comprise the following steps:
Step 1: take appropriate amount of sample dry under uniform temperature, to remove moisture;
Step 2: take dry sample in crucible, calcination under high temperature, with organics removal and volatile ingredient;
Step 3: be stirred in electric hot plate top heating edge after adding pyrophosphoric acid in the sample after calcination and react completely, reactant liquor is slowly poured in beaker filled with hot water, with Filter paper filtering, with watery hydrochloric acid, residue precipitation in beaker is washed funnel completely again, reusable heat water rinses and is precipitated to neutrality, to remove silicate;
Step 4: crucible filter paper being put into constant weight, at high temperature calcination is to constant weight, obtains zeyssatite.
2. assay method according to claim 1, it is characterized in that, the drying condition of sample is: dry 4h at 105 DEG C ± 2 DEG C.
3. assay method according to claim 1 or 2, is characterized in that, the calcination condition of dry sample is: calcination 1h at 850 DEG C ± 25 DEG C.
4. assay method according to claim 1 or 2, is characterized in that, the step removing silicate is: be stirred in 250 DEG C of electric hot plate top heating edge after adding 20mL pyrophosphoric acid in the sample after calcination and react completely; Slowly poured into by reactant liquor and filled in the 400mL beaker of 200mL hot water, filter while hot, with the watery hydrochloric acid of 0.1mol/L, residue precipitation in beaker is washed funnel completely, reusable heat water rinses and is precipitated to neutrality.
5. assay method according to claim 1 or 2, is characterized in that, after removing silicate, and final acquisition object SiO
2step be: crucible filter paper being put into constant weight, at 850 DEG C ± 25 DEG C, calcination is to constant weight.
6. assay method according to claim 1 or 2, wherein, calculates SiO as follows
2content (%)
In formula: m-take dry rear sample mass, g;
M
0empty crucible quality after-pre-burn, g;
M
1crucible and precipitation quality after-pre-burn, g.
7. according to any one of claim 1-6, measure method application in the detection of diatom ooze is analyzed of zeyssatite content.
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| CN201410625223.7A CN104316431B (en) | 2014-11-07 | 2014-11-07 | The assay method of kieselguhr content in a kind of diatom ooze wall material |
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| CN201410625223.7A CN104316431B (en) | 2014-11-07 | 2014-11-07 | The assay method of kieselguhr content in a kind of diatom ooze wall material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387479A (en) * | 2018-02-26 | 2018-08-10 | 浙江安联检测技术服务有限公司 | A kind of method of free silica content in detection air |
| CN112304800A (en) * | 2020-10-23 | 2021-02-02 | 成都兴蓉环保科技股份有限公司 | Method for determining organic matters in salt-containing solid waste |
| CN112763375A (en) * | 2021-03-02 | 2021-05-07 | 深圳市海龟梦新能源科技环保材料有限公司 | Method for determining content of diatomite in diatom ooze wall material |
Citations (2)
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| CN101334346A (en) * | 2008-08-05 | 2008-12-31 | 山东电力研究院 | Ingredient content analytical method for turbine blade salt deposition and scaling |
| CN101718664A (en) * | 2009-11-10 | 2010-06-02 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for measuring and calculating all iron content in imported iron ore |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334346A (en) * | 2008-08-05 | 2008-12-31 | 山东电力研究院 | Ingredient content analytical method for turbine blade salt deposition and scaling |
| CN101718664A (en) * | 2009-11-10 | 2010-06-02 | 天津出入境检验检疫局化矿金属材料检测中心 | Method for measuring and calculating all iron content in imported iron ore |
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| 中华人民共和国卫生部: "《GBZ/T192.4-2007工作场所空气中粉尘测定 第4部分：游离二氧化硅含量》", 18 June 2007 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387479A (en) * | 2018-02-26 | 2018-08-10 | 浙江安联检测技术服务有限公司 | A kind of method of free silica content in detection air |
| CN112304800A (en) * | 2020-10-23 | 2021-02-02 | 成都兴蓉环保科技股份有限公司 | Method for determining organic matters in salt-containing solid waste |
| CN112763375A (en) * | 2021-03-02 | 2021-05-07 | 深圳市海龟梦新能源科技环保材料有限公司 | Method for determining content of diatomite in diatom ooze wall material |
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Address after: Laoshan District, Qingdao three road 266000 Shandong city of Qingdao province No. 8 poly center 10 layer 1109 Patentee after: Qingdao Spring Gamay Diatom Ooze Technology Co., Ltd. Address before: 1305 room 182-6, Haier Road, Laoshan District, Shandong, Qingdao, 266000 Patentee before: Qingdao Spring Gamay Diatom Ooze Technology Co., Ltd. |