CN102323280A - Quality detection methods of pearl powder and application thereof - Google Patents
Quality detection methods of pearl powder and application thereof Download PDFInfo
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Abstract
The invention relates to a plurality of quality detection methods of pearl powder and application thereof. The quality detection methods of the pearl powder comprise any one or the combination of the following methods: 1, analyzing the pearl powder by an XRD (X-Ray Diffraction) diffraction method, wherein the content of a calcite phase in the pearl powder is less than or equal to 4.0 weight percent and the content of an aragonite phase in the pearl powder is more than or equal to 96.0 weight percent; and/or, 2, analyzing the pearl powder by DSC (Differential Scanning Calorimetry)/TGA (Thermal Gravimetric Analysis), wherein the content of organic matter in the pearl powder is in the range of 3.5 to 5.0 percent; and/or, 3, after heating the pearl powder to a temperature of 400 DEG C plus and minus 5 DEG C, analyzing the pearl powder by the XRD diffraction method so as to detect that in the pearl powder, the percentage content of the aragonite phase which is changed into calcite is in the range of 10.0 percent to 15.0 percent. By the quality detection methods provided by the invention, the pearl powder and the quality thereof can be identified, the pearl powder can be obviously distinguished from nacre powder and mixed powder, so that the controllability of the quality of the pearl powder is improved and the curative effect and the safety of the pearl powder are ensured.
Description
Technical field
The present invention relates to the quality determining method and the application thereof of pearl powder,, guarantee its curative effect and security to improve the controllability of pearl powder quality.
Background technology
Pearl is famous and precious ornament and famous and precious Chinese crude drug; The calcium activated, 18 seed amino acids, 30 various trace elements and the abundant vitamin B complex composition that contain 91-94%; Have clearing heat and detoxicating, drug effects such as yin-nourishing relieves dizziness, high fever, infantile convulsions, epilepsy, etc., the myogenic that makes eye bright, China is historical to its medication in existing more than 2000 year.
Pearl is divided into sea water pearls and fresh water pearl two big classes.China is the main place of production of pearl and pearl powder in the world, accounts for 75% of Gross World Product.At present; Only there are the high-grade pearl of 8-10% and 30% process level pearl can be processed into jewellery and handicraft in China fresh water pearl; Most pearls are difficult to be processed into artwork Ornament because of influenced by exterior appearance, size, aberration etc.; But be processed into pearl powder, as the raw material of multiple medicine, health products and cosmetics, to improve its added value.
The outward appearance of pearl is stratiform pearly-lustre color; X-ray diffraction analysis shows that it is the biologic inorganic mineral matter of crystalline state, is made up of the lime carbonate of aragonite (Aragonite) and two kinds of homogeneity different crystals of kalzit (Calcite) structure; Organic and aragonite, kalzit coexist as in the pearlite; Form inorganic organic complex, but do not present the crystal structure characteristic, make pearl have sparkling, beautiful sparkling and crystal-clear outward appearance of pearly-lustre and hard mechanical property.
Organic matter in the pearl mainly comprises amino acid, bioactive peptide, pearl protein etc.; And maybe be owing to the synergy of inorganic complex in the pearl and organic complex; Make pearl powder have beauty treatment, improve pharmaceutical properties such as eyesight, enhance immunity; Can be used for preparing medicine, health products and cosmetics etc., factor such as its biologically active and its composition and composition, processing method, microstructure (granular size, shape, distribution), noxious material (like lead, mercury, arsenic etc.) content, growth environment is relevant.
Along with growth in the living standard, pearl powder enjoys favor and attention in industries such as medicine, health food, cosmetics.The listing product comprise pearl powder, pearl oral liquid, pearl lozenge, precious chrysanthemum verticilum, Liushen Pills, piece and, pearl soap, pearl tooth-paste etc., and its application is also constantly being widened, the economic worth multiplication.At present, the output of China's pearl powder is 600 tons, and pearl powder and derived product annual value of production have reached 300,000,000 yuan, estimates that the output value of following 2-3 will be above 1,000,000,000 yuan.
Discover that the chemical composition of pearl shell internal layer (claim " nacre " again, the powder that its grinding and processing is formed is called " nacreous layer powder ") is similar with pearl powder, mainly contain lime carbonate, and contain several amino acids, but its content of amino acids is lower.Nacreous layer powder also can be done medicinal clinically, but its medical value and clinical efficacy are far below pearl powder.Yet nacreous layer powder is very similar with the appearance characteristics of pearl powder, is difficult to differentiate only according to naked eyes, and element composition analysis and optical microscope can't effectively detect and estimate its quality.Yet; The cost of nacreous layer powder is low; Often pretend to be pearl powder or sneak in the pearl powder and come into the market; Even still have like other outer appearnces powder (like shell powder, shell of seaear powder, talcum powder, Paris white etc.) be doped in the pearl powder or pretend to be pearl powder to come into the market, the mixed powder or the personation pearl powder of these matter time have a strong impact on consumer's health and safety, and hinder the sound development of pearl sector.
Yet the quality determining method of pearl powder and detection technique still belong to blank.Therefore; Be badly in need of research and set up quick, the easy pearl powder quality determining method of a cover; Be used to differentiate the true and false and its quality of evaluation of pearl powder; As the evaluation foundation that instructs, organizes production, acceptance of delivery and supervision and check, progressively standard pearl powder market and guarantee its security and validity promotes the sustainable and healthy development of pearl powder industry.
Summary of the invention
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, adopt the XRD diffraction approach to analyze the pearl powder, record the content≤4.0wt.% of its kalzit phase, aragonite phase content>=96.0wt.%.
Fresh water pearl and sea water pearls inorganic mainly comprises aragonite phase (Aragonite) and kalzit (calcite) mutually mutually, has six side's spherical calcium carbonate (Vaterite) thing phases individually.If from sample, detect other thing phase, then this sample of decidable is not pure pearl powder, should be Concha Margaritifera powder, or the mixed powder of mix Concha Margaritifera powder or other powders (like shell of seaear powder, talcum powder, Paris white etc.).
Pearl is the laminar crystal of oriented growth; Pearl powder after the pulverizing is laminar small crystals congeries; Its XRD powder diagram presents 001 diffraction structure characteristic; Promptly 001 diffraction peak is higher than 001 diffraction peak of the similar sample of non-structure, but the architectural feature of its 001 diffraction and relevant with it other diffraction peak thereof descends with the pearl powder smashing fineness.
Pearl and its parent clam shell; Particularly clam shell internal layer (nacre) all is the synusia shape crystal that piles up along 001 crystal plane orientation; Mechanical disintegration comprises that synusia is along splitting in the lamella and two kinds of failure modes of perpendicular slice direction fracture; The body of powder that generates is changed to spherical crystal block by little flat crystal block with broken course, and this transition process is relevant with factors such as housing and pearl mechanical properties.
The clam shell housing is made up of cuticula, prismatic layer (this layer contains kalzit) and nacre.Pearl itself does not contain the kalzit phase, and its kalzit is from being formed through phase transformation by aragonite in the mechanical processing process.
In the optimal technical scheme of the present invention, the crystallographic system of aragonite thing phase is a quadrature.
In the optimal technical scheme of the present invention, the space group of aragonite thing phase is pmcn.
In the optimal technical scheme of the present invention; The cell parameter of aragonite thing phase is a:
b:
c:
Z=4, D (calc)=2.92.
In the optimal technical scheme of the present invention, the crystallographic system of kalzit phase is tripartite.
In the optimal technical scheme of the present invention, the space group of kalzit phase is R
3-CH.
In the optimal technical scheme of the present invention; The cell parameter of kalzit phase is
Z=6, D=2.73.
In the optimal technical scheme of the present invention, the test condition of XRD diffraction approach does, the CuKarf radiation, and DS/SS:1 ° of RS 0.2mm, diffracted ray bondstone China ink monochromator is removed the Kbata radiation, and power is not less than 1.6 kilowatts, and the step scanning mode is gathered the diffraction experiment data.
In the optimal technical scheme of the present invention, the preparation method of XRD diffraction approach analytic sample comprises any or its combination of following method:
1) directly presses the powdery diffractometry sample preparation methods, be pressed in sample powder on the specimen holder of XRD diffractometer, again it is inserted the diffractometer test and collects experimental data; And/or
2) accurately measure the construction coefficient sample, powdered samples is processed 1% suspending liquid earlier, drops on the tabular sample panel with dropper, inserts the XRD diffractometer behind the airing and detects and collect experimental data.
In the optimal technical scheme of the present invention, the XRD diffraction approach is measured the gained diffraction data and is carried out data processing with the Jade9 software package.
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, adopt DSC/TGA to analyze the pearl powder, recording its organic content is 3.5-5.0%.
In the optimal technical scheme of the present invention, the content of organic matter in the pearl meal is 4.3-4.6%.
In the optimal technical scheme of the present invention, the content of organic matter in the pearl fine powder is 4.0-4.3%.
In the optimal technical scheme of the present invention, the content of organic matter in the pearl micropowder is 3.5-4.0%.
In the optimal technical scheme of the present invention, said DSC/TGA curve test method comprises the steps:
A) with thermogravimetric analyzer (DSC/TGA) start preheating 30 minutes, connect air;
B) balance reading makes zero after stablizing, and opens stove and takes off dress appearance, with α-Al
2O
3The crucible 10-15mg testing sample of packing into is put back to, and shuts stove;
C) treat that balance reading is stable after, be warming up to 800 ℃ with the speed of 10 ℃/min, measure the TG/DTA curve, will detect data file and deposit, and utilize the instrument software deal with data.
The oxygenolysis temperature of organic matter is far below the decomposition temperature of inorganic mineral phase in the pearl powder.Thermogravimetric analysis can quantize to write down pearl delicately and be aspects such as the oxygenolysis of amorphous organic matter in air atmosphere, phase transformation, decomposable process, to obtain information such as its content of organic matter, decomposition temperature.
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, adopt the XRD diffraction analysis after pearl powder is heated to 400 ℃ ± 5 ℃, detect the percentage composition that pearl powder Chinese stone becomes kalzit mutually.
In the optimal technical scheme of the present invention, adopt the XRD diffraction analysis after pearl powder is heated to 400 ℃ ± 5 ℃, the percentage composition that is become kalzit by aragonite mutually is 10.0%-15.0%.
In the optimal technical scheme of the present invention, adopt the XRD diffraction analysis after shell powder is heated to 400 ℃ ± 5 ℃, the percentage composition that is become kalzit by aragonite mutually does, 25.0%＜become percentage composition＜60.0% of kalzit mutually by aragonite.
In the optimal technical scheme of the present invention, adopt the XRD diffraction analysis after mixed powder is heated to 400 ℃ ± 5 ℃, the percentage composition that is become kalzit by aragonite mutually does, 15.0%＜become percentage composition＜25.0% of kalzit mutually by aragonite.
In the optimal technical scheme of the present invention; The analysis condition of the hot phase transformation of sample does in the XRD diffraction approach, and diffractometer rises to 400 ℃ ± 5 ℃ with the speed of 100 ℃/min, is incubated 10 minutes; Reduce to normal temperature with the speed of 100 ℃/min again, at the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens.
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, 1) adopt XRD diffraction analysis pearl powder, record the content≤4.0wt.% of its kalzit phase, aragonite phase content>=96.0wt.%; And/or
2) adopt DSC/TGA to analyze the pearl powder, recording its organic content is 3.5-5.0%.
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, 1) after being heated to 400 ℃ ± 5 ℃, the pearl powder adopts the XRD diffraction analysis, record the percentage composition 10.0%-15.0% that pearl powder Chinese stone becomes kalzit mutually; And/or
2) adopt DSC/TGA to analyze the pearl powder, recording its organic content is 3.5-5.0%.
In the optimal technical scheme of the present invention; The analysis condition of the hot phase transformation of sample does in the XRD diffraction approach, and diffractometer rises to 400 ℃ ± 5 ℃ with the speed of 100 ℃/min, is incubated 10 minutes; Reduce to normal temperature with the speed of 100 ℃/min again, at the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens.
The object of the present invention is to provide a kind of quality determining method of pearl powder, it is characterized in that, 1) adopt the XRD diffraction approach to analyze the pearl powder, record the content≤4.0wt.% of its kalzit phase, aragonite phase content>=96.0wt.%; And/or
2) adopt the XRD diffraction analysis after the pearl powder is heated to 400 ℃ ± 5 ℃, record the percentage composition 10.0%-15.0% that pearl powder Chinese stone becomes kalzit mutually; And/or
3) adopt DSC/TGA to analyze the pearl powder, recording its organic content is 3.5-5.0%.
In the optimal technical scheme of the present invention; The analysis condition of the hot phase transformation of sample does in the XRD diffraction approach, and diffractometer rises to 400 ℃ ± 5 ℃ with the speed of 100 ℃/min, is incubated 10 minutes; Reduce to normal temperature with the speed of 100 ℃/min again, at the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens.
For clear statement protection scope of the present invention, the present invention carries out as giving a definition term:
Pearl meal according to the invention is meant that mean grain size is that
degree of orientation p001 is the pearl powder of 0.5-0.7.
Pearl fine powder according to the invention is meant that mean grain size is that
degree of orientation p001 is the pearl powder of 0.7-0.8.
Pearl micropowder according to the invention is meant that mean grain size is that
degree of orientation p001 is the pearl powder of 0.8-1.0.
" mother-of-pearl " of the present invention; Another name pearl tree peony, pearl oyster, natural pearls are female, jewel is female, and these article are the shell of Unionidae animal hydriopsis cumingii Hyriopsis cumingii (Lea), cristaria plicata Cristaria plicata (Leach) or Pteriidae animal Pinctada martensii Pteria martensii (Dunker).Fleshing, cleaning, drying.
" pearl shell internal layer " of the present invention claimed " nacre " again, and the powder that its grinding and processing is formed is called " nacreous layer powder ".
" Concha Margaritifera powder " of the present invention claimed " shell powder " again, is meant that the shell of Unionidae animal hydriopsis cumingii, cristaria plicata, Pteriidae animal Pinctada martensii is removed impurity, and the powder that forms is pulverized in processing.
" mixed powder " of the present invention is meant the adulterated flour that in pure pearl powder, adds other non-pearl powder powder (like shell powder, talcum powder, flour etc.) and get.
" XRD diffraction approach " of the present invention claimed " XRD diffraction analysis method ", " XRD analysis method " again; Adopt the XRD diffraction result of XRD powder diffractometer working sample, with information such as the thing phase composition of obtaining sample and abundance thereof, micromechanism information (crystal block size, shape, structure), crystallography parameter, crystal parameterses.
The analysis condition of the hot phase transformation of sample does in the XRD diffraction approach of the present invention; Diffractometer is warming up to 400 ℃ ± 5 ℃ with the speed of 100 ℃/min; Be incubated 10 minutes, the speed with 100 ℃/min is cooled to normal temperature again, at the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens.
DSC/TGA method of the present invention is claimed thermogravimetry, DSC/TGA curve test method again; This method adopts the thermogravimetric analyzer detection to follow the tracks of factors such as the heat absorption of material heat temperature raising process, heat release, mass change; Quantize fast to obtain the decomposition temperature and the content information thereof of amalyzing substances, and have characteristics such as sensitivity, repeatability be good.
The preparation method of pearl powder according to the invention comprises the steps: pearl is cleaned, and as required, adopts mechanical-physical methods such as ball milling, air-flow are pulverized, water flies to pulverize, to make the pearl powder of different fineness.
The preparation method of Concha Margaritifera powder according to the invention can take any or its combination of following method,
1) mother-of-pearl is cleaned, as required, adopted mechanical-physical methods such as ball milling, air-flow are pulverized, water flies to pulverize, to make the Concha Margaritifera powder of different fineness; And/or
2) with mother-of-pearl with buck (like NaOH, potassium hydroxide, soda mint etc.) immersion treatment after; Taking-up is clean with flushing with clean water, after drying or drying, as required; Adopt mechanical-physical methods such as ball milling, air-flow are pulverized, water flies to pulverize, to make the Concha Margaritifera powder of different fineness; And/or
3) with emery wheel the outer cuticula of mother-of-pearl is removed after, as required, adopt mechanical-physical methods such as ball milling, air-flow are pulverized, water flies to pulverize, to make the Concha Margaritifera powder of different fineness.
The preparation method of mixed powder of the present invention does, pearl powder is evenly mixed in required ratio with Concha Margaritifera powder or other powder and gets.
Except as otherwise noted, percentage composition of the present invention is a weight percentage.
The detection method of pearl powder of the present invention comprises XRD analysis method and DSC/TGA curve test method, and its method of testing and test condition comprise:
1, XRD analysis method
(1) instrument: XRD powder diffractometer, B-B diffraction geometry THET-THET angular instrument, angular instrument resolution, halfwidth (FHWM)＜0.07 ° 2 θ that about 28 ° no wideization of instrument intrinsic standard models of 2 θ (SRM1976 or srmLaB6) are measured.
(2) test condition
The CuKarf radiation, DS/SS:1 ° of RS 0.2mm, diffracted ray bondstone China ink monochromator is removed the Kbata radiation, and power is not less than 1.6 kilowatts, and the step scanning mode is gathered the diffraction experiment data.
(3) sample preparation methods: 1. directly press the powdery diffractometry sample preparation methods, be pressed in sample powder on the specimen holder of XRD diffractometer, again it is inserted the diffractometer test and collects experimental data; And/or
2. accurately measure the construction coefficient sample, powdered samples is processed 1% suspending liquid earlier, drops on the tabular sample panel with dropper, inserts the detection of XRD diffractometer behind the airing and collects experimental data, will record diffraction data and carry out data processing with the Jade9 software package.
2, the DSC/TGA curve test method comprises the steps:
A) with thermogravimetric analyzer (DSC/TGA) start preheating 30 minutes, connect air;
B) balance reading makes zero after stablizing, and opens stove and takes off dress appearance, with α-Al
2O
3The crucible 10-15mg testing sample of packing into is put back to, and shuts stove;
C) treat that balance reading is stable after, be warming up to 800 ℃ with the speed of 10 ℃/min, measure the TG/DTA curve, data file deposit, and utilize instrument software processing and detecting data.
Another object of the present invention is to provide the quality determining method of pearl powder to be used for detecting or control the application of the quality of pearl powder or its medicine or its health products or its cosmetics.
Description of drawings
The XRD diffraction testing result of Fig. 1 pearl meal, pearl fine powder, pearl micropowder and non-structure powder;
The DSC/TGA testing result of Fig. 2 pearl parent shell powder;
The DSC/TGA testing result of Fig. 3 pearl powder;
Fig. 4 Concha Margaritifera powder is at the XRD phase transformation comparing result of 400 ℃ of insulations after 10 minutes;
Fig. 5 pearl powder is at the XRD phase transformation comparing result of 400 ℃ of insulations after 10 minutes;
Fig. 6 mixed powder is at the XRD phase transformation comparing result of 400 ℃ of insulations after 10 minutes;
The XRD powder diffraction analysis result of the commercially available pearl powder of Fig. 7 (real is Concha Margaritifera powder);
The hot phase transformation analysis result of XRD diffraction of the commercially available pearl powder of Fig. 8 (real is Concha Margaritifera powder);
The DSC/TGA testing result of the commercially available pearl powder of Fig. 9 (real is Concha Margaritifera powder);
The XRD powder diffraction analysis result of the commercially available pearl powder of Figure 10 (real is Concha Margaritifera powder);
The hot phase transformation analysis result of XRD diffraction of the commercially available pearl powder of Figure 11 (real is Concha Margaritifera powder);
The DSC/TGA testing result of the commercially available pearl powder of Figure 12 (real is Concha Margaritifera powder);
The XRD powder diffraction analysis result of Figure 13 pearl powder;
The hot phase transformation analysis result of the XRD diffraction of Figure 14 pearl powder;
The DSC/TGA testing result of Figure 15 pearl powder.
The XRD powder diffraction analysis result of Figure 16 mixed powder;
The hot phase transformation analysis result of the XRD diffraction of Figure 17 mixed powder;
The DSC/TGA testing result of Figure 18 mixed powder;
The XRD powder diffraction analysis result of Figure 19 Taiwan pearl powder;
The hot phase transformation analysis result of the XRD diffraction of Figure 20 Taiwan pearl powder;
The DSC/TGA testing result of Figure 21 Taiwan pearl powder.
Embodiment
Below will combine embodiment to specify the present invention, embodiments of the invention only are used to technical scheme of the present invention is described, and non-limiting essence of the present invention.
Embodiment 1The XRD diffraction approach detects the quality of pearl powder, Concha Margaritifera powder and mixed powder
Test sample or purchase various trade mark pearl powders perhaps adopts to be derived from cultured pearl and the parent clam shell thereof that Zhuji, Zhejiang Province produces, according to preparation method's preparation of the present invention and get.
Adopt XRD diffraction approach analytic sample, confirm to differentiate and detect the index of pearl powder quality through comparative studies.
1, XRD analysis method and test condition
(1) instrument: XRD powder diffractometer, B-B diffraction geometry THET-THET angular instrument, angular instrument resolution, halfwidth (FHWM)＜0.07 ° 2 θ that about 28 ° no wideization of instrument intrinsic standard models of 2 θ (SRM1976 or srmLaB6) are measured.
(2) test condition
The CuKarf radiation, DS/SS:1 ° of RS 0.2mm, diffracted ray bondstone China ink monochromator is removed the Kbata radiation, and power is not less than 1.6 kilowatts, and the step scanning mode is gathered the diffraction experiment data.
Sample preparation methods: 1. powdered sample is directly pressed the powdery diffractometry sample preparation methods, is pressed in powder on the specimen holder that instrument provides, and inserts the diffractometer test; And/or
2. accurately measure the construction coefficient sample, powdered samples is processed 1% suspending liquid earlier, drops on the tabular sample panel with dropper, inserts instrument behind the airing and collects experimental data.
(3) diffraction data that records is carried out data processing with the Jade9 software package, the result sees table 1.
Visible by table 1, adopt the analysis of XRD diffraction approach, the content≤4.0wt.% of kalzit phase in the pearl powder compares than Concha Margaritifera powder or mixed powder, and its kalzit content is obviously on the low side; Aragonite phase content>=96.0wt.% in the pearl powder compares than Concha Margaritifera powder or mixed powder, and its aragonite phase content is obviously higher.In view of the above, can differentiate pearl powder and quality thereof, and can pearl powder and Concha Margaritifera powder, mixed powder significantly be distinguished, can be with it separately as the quality detecting index of pearl powder.
Embodiment 2Thermal analysis system detects the quality of pearl powder, Concha Margaritifera powder and mixed powder
1, thermogravimetry and test condition
A) start preheating thermogravimetric analyzer (DSC/TGA) is 30 minutes, connects air;
B) treat that balance reading makes zero after stable, open stove and take off dress appearance, with α-Al
2O
3The crucible 10-15mg testing sample of packing into is put back to, and shuts stove;
C) treat that balance reading is stable after, be warming up to 800 ℃ with the heating rate of 10 ℃/min from room temperature, measure the TG/DTA curve, data file deposit, and utilize instrument software processing and detecting data, the result sees table 1.
Visible by table 1, analyze through DSC/TG, to compare with Concha Margaritifera powder, mixed powder, the content of organic matter in the pearl powder is 3.5-5.0%, and is higher relatively, wherein, the content of organic matter in the pearl meal is 4.3-4.6%; The content of organic matter in the pearl fine powder is 4.0-4.3%; The content of organic matter in the pearl micropowder is 3.5-4.0%.In view of the above, can differentiate pearl powder and quality thereof, and can pearl powder and Concha Margaritifera powder, mixed powder significantly be distinguished, can be with it separately as the quality detecting index of pearl powder.
Embodiment 3The quality of differentiating pearl powder, Concha Margaritifera powder and mixed powder is analyzed in the hot phase transformation of sample in the XRD diffraction approach
The analysis condition of the hot phase transformation of sample is in the XRD diffraction approach: after sample is inserted diffractometer; Speed with 100 ℃/min rises to 400 ℃ ± 5 ℃, is incubated 10 minutes, reduces to normal temperature with the speed of 100 ℃/min again; At the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens, the result sees table 1.
The quality testing result of table 1 pearl powder, Concha Margaritifera powder, mixed powder
Visible by table 1, after being heated to 400 ℃ ± 5 ℃, adopts pearl powder the XRD diffraction analysis, and its testing result and Concha Margaritifera powder, mixed powder exist significantly to be distinguished, and the percentage composition that becomes kalzit mutually by aragonite in the pearl powder is 10.0%-15.0%; The percentage composition that becomes kalzit mutually by aragonite in the shell powder does, 25.0%＜become percentage composition＜60.0% of kalzit mutually by aragonite; The percentage composition that becomes kalzit mutually by aragonite in the mixed powder does, 15.0%＜become percentage composition＜25.0% of kalzit mutually by aragonite.In view of the above, can differentiate pearl powder and quality thereof, and can pearl powder and Concha Margaritifera powder, mixed powder significantly be distinguished, can be with it separately as the quality detecting index of pearl powder.
The quality testing result of embodiment 4 different-grain diameter pearl powders
The pearl in Zhuji is originated from employing; Make the pearl powder of required particle diameter according to preparation method of the present invention; Comprise pearl meal (mean grain size is 0.5-0.7 for
degree of orientation p001), pearl fine powder (mean grain size is 0.7-0.8 for
degree of orientation p001), pearl micropowder (mean grain size is 0.8-1.0 for
degree of orientation p001); Detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Fig. 1.
Visible by Fig. 1, the diffractogram of superfine pearl powder and non-structure standard powder diagram synoptic diagram are the most approaching, and the structure degree of three kinds of different fineness pearl powders is successively decreased from bottom to top, and the diffraction peak of kalzit phase has only the strong peak of leading to detect, and content is very low.Lower frame has marked the relative intensity of each diffraction peak among Fig. 1.
Embodiment 5The hot analysis result comparative studies of pearl powder and Concha Margaritifera powder
The pearl and the pearl shell thereof in Zhuji originated from employing, makes the pearl powder or the Concha Margaritifera powder of required particle diameter according to preparation method of the present invention, detects according to thermogravimetry of the present invention and testing conditions thereof, and the result sees Fig. 2-Fig. 3.
Visible by Fig. 2-Fig. 3, the organic matter oxidative pyrolysis pattern in air atmosphere in pearl powder and its parent shell powder is similar, on pyrolysis oxidizing temperature and organic weight loss, there are differences, and the organic total amount in the pearl powder is apparently higher than its parent shell powder.
Embodiment 6The hot phase transformation analysis of sample in the pearl powder XRD diffraction approach
The pearl and the pearl shell thereof in Zhuji originated from employing; Make pearl powder, Concha Margaritifera powder and the mixed powder of required particle diameter according to preparation method of the present invention; Detect according to hot phase transformation analytic approach of sample and testing conditions thereof in the XRD diffraction approach of the present invention, the result sees Fig. 4-Fig. 6.
Visible by Fig. 4-Fig. 6, after being heated to 400 ℃ ± 5 ℃, adopts pearl powder the XRD diffraction analysis, and its result and Concha Margaritifera powder, mixed powder exist significantly to be distinguished, and the percentage composition that becomes kalzit mutually by aragonite in the pearl powder is 11.9%; The percentage composition that becomes kalzit mutually by aragonite in the shell powder is 35.0%; The percentage composition that becomes kalzit mutually by aragonite in the mixed powder is 19.2%.In view of the above, can differentiate pearl powder and quality thereof, and can pearl powder and Concha Margaritifera powder, mixed powder significantly be distinguished, can be with it separately as the quality detecting index of pearl powder.
Embodiment 7The testing result of commercially available pearl powder (real is Concha Margaritifera powder)
Purchase commercially available pearl powder, detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Fig. 7-Fig. 9.
1, the XRD diffraction analysis result of sample has detected alpha-quartz, and promptly other thing phases determine that it is Concha Margaritifera powder.
2, to record its kalzit content be 35.0wt.% to the hot phase transformation analysis of the XRD of sample, determines that it is Concha Margaritifera powder.
3, to record its content of organic matter be 3.4wt.% to the thermogravimetric analysis result of sample, determines that it is Concha Margaritifera powder.
Embodiment 8The testing result of commercially available pearl powder (real is Concha Margaritifera powder)
Purchase commercially available pearl powder, detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Figure 10-Figure 12.
1, the XRD powder diffraction analysis result of sample records its kalzit content above 4.0%, determines that it is Concha Margaritifera powder.
2, the hot phase transformation analysis result of the XRD of sample records its kalzit phase content up to more than the 50.wt.0%, determines that it is Concha Margaritifera powder.
3, the thermogravimetric analysis result of sample records its content of organic matter＜3.6wt.%, determines that it is Concha Margaritifera powder.
Embodiment 9The testing result of pearl powder
The pearl in Zhuji is originated from employing; Make the pearl powder of required particle diameter according to preparation method of the present invention; Detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Figure 13-Figure 15.
1, the XRD analysis of sample (not hot phase transformation is handled preceding) records its kalzit content 1.2wt.%, determines that it is pearl powder.
2, the hot phase transformation analysis of the XRD of sample records kalzit content 10.6wt%, determines that it is pearl powder.
3, the thermogravimetric analysis result of sample records its content of organic matter 4.6wt.%, determines that it is Concha Margaritifera powder.
Embodiment 10The testing result of mixed powder
Purchase commercially available pearl powder, detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Figure 16-Figure 18.
Its each item of analysis-by-synthesis is picked up the survey data, determines that it is the mixed powder that contains the 10-20wt.% shell powder.
Embodiment 11The testing result of Taiwan pearl powder
Purchase commercially available Taiwan pearl powder, detect according to hot phase transformation analysis of sample and thermogravimetry and testing conditions thereof in XRD diffraction approach of the present invention, the XRD diffraction approach, the result sees Figure 19-Figure 21.
Its each item of analysis-by-synthesis is picked up the survey data, judges that it contains the mixed powder of the 20wt.% shell powder of having an appointment.
Claims (10)
1. the quality determining method of a pearl powder is characterized in that, comprises any or its combination of following method:
1) adopts the XRD diffraction approach to analyze the pearl powder, record the content≤4.0wt.% of its kalzit phase, aragonite phase content>=96.0wt.%; And/or
2) adopt the XRD diffraction analysis after the pearl powder is heated to 400 ℃ ± 5 ℃, record the percentage composition 10.0%-15.0% that pearl powder Chinese stone becomes kalzit mutually; And/or
3) adopt DSC/TGA to analyze the pearl powder, recording its organic content is 3.5-5.0%.
2. quality determining method according to claim 1; The crystallographic system of said aragonite thing phase is a quadrature; Preferred its space group is pmcn; More preferably its cell parameter is a:
b:
c:
Z=4, D (calc)=2.92.
3. quality determining method according to claim 1 and 2, the crystallographic system of said kalzit phase are tripartite, and preferably its space group is R
3-CH, more preferably its cell parameter does
Z=6, D=2.73.
4. according to each described quality determining method of claim 1-3, the test condition of XRD diffraction approach is the CuKarf radiation; DS/SS:1 ° of RS 0.2mm; Diffracted ray bondstone China ink monochromator is removed the Kbata radiation, and power is not less than 1.6 kilowatts, and the step scanning mode is gathered the diffraction experiment data.
5. according to each described quality determining method of claim 1-4, the preparation method of XRD diffraction approach analytic sample comprises:
1) directly presses the powdery diffractometry sample preparation methods, be pressed in sample powder on the specimen holder of XRD diffractometer, again it is inserted the diffractometer test and collects experimental data; And/or
2) accurately measure the construction coefficient sample, powdered samples is processed 1% suspending liquid earlier, drops on the tabular sample panel with dropper, inserts the XRD diffractometer behind the airing and detects and collect experimental data.
6. according to each described quality determining method of claim 1-5, it is characterized in that adopt the XRD diffraction analysis after pearl powder is heated to 400 ℃ ± 5 ℃, the percentage composition that is become kalzit by aragonite mutually is 10.0%-15.0%.
7. according to each described quality determining method of claim 1-6, said DSC/TGA curve test method comprises the steps:
A) with thermogravimetric analyzer (DSC/TGA) start preheating 30 minutes, connect air;
B) balance reading makes zero after stablizing, and opens stove and takes off dress appearance, with α-Al
2O
3The crucible 10-15mg testing sample of packing into is put back to, and shuts stove;
C) treat that balance reading is stable after, be warming up to 800 ℃ with the speed of 10 ℃/min, measure the TG/DTA curve, will detect data file and deposit, and utilize the instrument software deal with data.
8. quality determining method according to claim 7; It is characterized in that; The content of organic matter in the pearl meal is 4.3-4.6%, and the content of organic matter in the preferred pearl fine powder is 4.0-4.3%, and more preferably the content of organic matter in the pearl micropowder is 3.5-4.0%.
9. according to each described quality determining method of claim 1-8; It is characterized in that; The analysis condition of the hot phase transformation of sample does in the XRD diffraction approach, and diffractometer rises to 400 ℃ ± 5 ℃ with the speed of 100 ℃/min, is incubated 10 minutes; Reduce to normal temperature with the speed of 100 ℃/min again, at the diffraction data of 15 ℃-70 ℃ 2 θ scope collected specimens.
10. the quality determining method of each described pearl powder of claim 1-9 is used for detecting or control the application of the quality of pearl powder or its medicine or its health products or its cosmetics.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110121080A CN102323280A (en) | 2011-05-11 | 2011-05-11 | Quality detection methods of pearl powder and application thereof |
| CN201210147099.9A CN102706911B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof |
| CN201210146928.1A CN102721713B (en) | 2011-05-11 | 2012-05-11 | Thermal analysis system detects method and the application thereof of pearl powder quality |
| CN201210146088.9A CN102798641B (en) | 2011-05-11 | 2012-05-11 | Quality detection method of pearl powder and application of quality detection method |
| CN201210145993.2A CN102798640B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by XRD (X-Ray Diffraction) and application thereof |
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| CN201210146928.1A Active CN102721713B (en) | 2011-05-11 | 2012-05-11 | Thermal analysis system detects method and the application thereof of pearl powder quality |
| CN201210145993.2A Active CN102798640B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by XRD (X-Ray Diffraction) and application thereof |
| CN201210147099.9A Expired - Fee Related CN102706911B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof |
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| CN201210145993.2A Active CN102798640B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by XRD (X-Ray Diffraction) and application thereof |
| CN201210147099.9A Expired - Fee Related CN102706911B (en) | 2011-05-11 | 2012-05-11 | Method for detecting quality of pearl powder by using thermal transformation hemodynamic difference combined with X-ray diffraction (XRD) and application thereof |
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| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
| CN106896033A (en) * | 2017-04-26 | 2017-06-27 | 安徽理工大学 | A kind of method of the content of organic matter in measure gangue |
| CN109444186A (en) * | 2018-12-25 | 2019-03-08 | 浙江大学 | A kind of pearl powder X-ray diffraction differential method |
| CN110031486A (en) * | 2019-04-18 | 2019-07-19 | 广东海洋大学 | A kind of method of quick identification seawater and fresh water pearl powder |
| CN112986040A (en) * | 2019-12-12 | 2021-06-18 | 中国科学院大连化学物理研究所 | Quantitative detection method for surfactant in nano catalyst |
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| CN102323280A (en) * | 2011-05-11 | 2012-01-18 | 浙江长生鸟珍珠生物科技有限公司 | Quality detection methods of pearl powder and application thereof |
| CN103411861B (en) * | 2013-08-23 | 2015-09-16 | 中国检验检疫科学研究院 | The assay method of a kind of pearl powder and oyster shell whiting reunion index |
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| JP2006118923A (en) * | 2004-10-20 | 2006-05-11 | Tohoku Univ | Nondestructive inspection method for quality level of pearl oyster |
| CN101620176B (en) * | 2009-06-10 | 2011-01-12 | 钱国英 | Method for distinguishing pearl powders from shell powders |
| WO2012090043A1 (en) * | 2010-12-29 | 2012-07-05 | Jubilant Life Sciences Limited | Novel solid state forms of azilsartan medoxomil and preparation thereof |
| CN102323280A (en) * | 2011-05-11 | 2012-01-18 | 浙江长生鸟珍珠生物科技有限公司 | Quality detection methods of pearl powder and application thereof |
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- 2012-05-11 CN CN201210146088.9A patent/CN102798641B/en active Active
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323470A (en) * | 2013-01-13 | 2013-09-25 | 赵景红 | Toilet powder and detection method of asbestos in talcum powder |
| CN106896033A (en) * | 2017-04-26 | 2017-06-27 | 安徽理工大学 | A kind of method of the content of organic matter in measure gangue |
| CN109444186A (en) * | 2018-12-25 | 2019-03-08 | 浙江大学 | A kind of pearl powder X-ray diffraction differential method |
| CN110031486A (en) * | 2019-04-18 | 2019-07-19 | 广东海洋大学 | A kind of method of quick identification seawater and fresh water pearl powder |
| CN112986040A (en) * | 2019-12-12 | 2021-06-18 | 中国科学院大连化学物理研究所 | Quantitative detection method for surfactant in nano catalyst |
Also Published As
| Publication number | Publication date |
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| CN102706911A (en) | 2012-10-03 |
| CN102798640A (en) | 2012-11-28 |
| CN102706911B (en) | 2014-10-01 |
| CN102798640B (en) | 2015-02-11 |
| CN102721713B (en) | 2015-11-18 |
| CN102798641B (en) | 2015-01-07 |
| CN102798641A (en) | 2012-11-28 |
| CN102721713A (en) | 2012-10-10 |
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