CN110926904A - Wheat imperfect grain standard sample and preparation method thereof - Google Patents
Wheat imperfect grain standard sample and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a standard sample of imperfect wheat grains and a preparation method thereof. The imperfect wheat grain standard sample is prepared by embedding decayed grains, scab grains, damaged grains, germinated grains and mildewed grains in organic resin. The standard sample of imperfect wheat grains prepared by the invention has good uniformity and stability, is easy to store, has the effective period of more than 10 years, fills the blank of manufacturing the standard sample of imperfect wheat grains at home and abroad, and standardizes the inspection work of the project of imperfect wheat grains in China.
Description
Technical Field
The invention belongs to the technical field of preparation of plant seed standard samples, and particularly relates to a standard sample of imperfect wheat grains and a preparation method thereof.
Background
China is the largest producing and consuming country of wheat in the world and is also the international trade and big country of wheat. In international grain trade, grain price is directly hooked with grain grade, and the content of indexes such as imperfect grains directly influences economic benefit. Therefore, the work of checking the imperfect wheat grain project is an indispensable part of maintaining the interests of the country and the enterprise. At present, the inspection of imperfect wheat grain items is sensory inspection, and the inspection result is directly influenced by human factors such as experience of inspection technicians, eye light and the like. Because of no assistance of a precise instrument, the actual conditions of the broken degree and the mildewing degree of the wheat and the like in the imperfect grain inspection all generate errors due to different inspectors, sometimes, the errors directly cause different results to seriously affect the working quality, and the inspection work of imperfect grain projects needs matched standard samples; in addition, in the aspect of laboratory quality management, because the subjective error of the imperfect wheat grain inspection is large, no matched standard sample exists, the laboratory quality control activity cannot be well carried out, and the matched imperfect grain standard sample is very necessary to be formulated.
A standard sample is a physical standard having one or more performance characteristics and approved by a technical certification and standardization authority. The standard sample is an important technical means for scientifically establishing a technical standard and effectively implementing the technical standard, controlling and improving the quality of industrial and agricultural products, ensuring the food safety, guaranteeing the personal health and the environmental quality and the like. The standard sample is an organic component of the whole standardization work, and is a substance embodiment which needs to be quantitatively or qualitatively described by the content requirements of the literal standard by using the standard sample, and plays an important role in ensuring the implementation of the standard. It is commonly used for quality assessment and control of analytical test substances, calibration of analytical instruments, assessment validation of analytical methods, comparison of analytical data, product quality assessment, assessment of the skill level of inspectors, technical arbitration, and the like. Due to the advantages of special uniformity, stability, intuition, accuracy and the like, research work on standard samples is getting more and more concerned by experts in various related fields.
Therefore, the standard sample undoubtedly plays an important role in the imperfect wheat grain project inspection work, is a specific explanation of imperfect grain standard definition, uniformly judges the eyesight and reduces the subjective error of sensory inspection; in addition, the imperfect wheat grain standard sample provides a reliable and scientific material basis for developing quality control activities in the inspection field, is favorable for laboratory quality control, is favorable for improving the laboratory quality management level, and reduces the risk of accuracy of laboratory inspection results. The work of making a standard sample of imperfect grains of wheat is very significant.
The research work of the standard samples in China starts late, starting from the 50 s of the 20 th century, and the management of the production, distribution and application of the standard samples is brought into the scope of standardized management in the early 80 s. In China, the preparation and development of standard samples are taken as a new technology, firstly, the technology is carried out in the fields of metallurgy, nonferrous metals and the like, then, the technology is developed into the fields of chemistry, fuel, food and the like, but the research on sensory standard samples of agricultural products is less. At present, the manufacturing work of standard samples does not relate to the field of sensory inspection of imperfect grains of grains (including wheat), no research institution is involved in the manufacturing and development work of the standard samples of the imperfect grains of grains, and in the departments in charge of import and export of the quality inspection of the grains in China, professional persons specialized in the quality inspection and particularly the sensory inspection are not too many, inspection experts in the field are more flexible, many of the working posts are specially operated by non-professional persons of the quality of the grains, in the specific inspection process, comparison is mostly carried out according to standard character definitions or comparison inspection is carried out according to partially referable pictures, in addition, the partial imperfect grains have different standards and the definitions have different conditions. These factors contribute to the accuracy of the imperfect kernel project test results to a great extent, and also contribute to the incomparable test results among laboratories.
Disclosure of Invention
The invention aims to provide a standard sample of imperfect wheat grains and a preparation method thereof.
The imperfect wheat grain standard sample is prepared by embedding decayed grains, scab grains, damaged grains, germinated grains and mildewed grains in organic resin.
The embedding operation comprises the following steps:
(1) manufacturing a mould, and uniformly spraying the bright paint on the surface of the mould;
(2) cleaning the mold and then assembling an outer mold;
(3) adding the filler into the organic resin, uniformly stirring, adding the ingredients, and uniformly stirring to prepare an embedding solution;
(4) pouring the embedding liquid into a mold, and shaking the mold to ensure that the embedding liquid in the mold flows uniformly;
(5) putting the seeds into an embedding liquid, and removing the mold after the embedding liquid is completely solidified;
(6) and (5) grinding and polishing the product.
The bright paint comprises the following components in parts by weight: 50-70 parts of acrylic resin, 10-20 parts of talcum powder, 3-5 parts of pure acrylic emulsion and 3-5 parts of phenyldiisocyanate tripolymer.
The organic resin comprises the following components in parts by weight: 60-80 parts of polyethylene glycol, 20-30 parts of transparent urea-formaldehyde resin and 20-30 parts of epoxy resin.
The filler is barite powder, is prepared by crushing, grinding and sieving barite powder with a sieve of 400-one and 500-one, and the adding proportion is 3-12% of the mass of the organic resin.
The natural gunite is a fluosilicate, whose mineral characteristics have been studied by Zhang Hui Ming et al, and is basically a granular aggregate, colorless, itself having glass luster, translucent to transparent, soluble in nitric acid, sparingly soluble in hydrochloric acid, gunite (3 CaO.2SiOx)2·CaF2) It is a monoclinic crystal, and its local structure is characterized by that two silicon-oxygen tetrahedrons are connected by means of bridge oxygen, and at the same time, they are connected with four calcium octahedrons in the mode of sharing edge or corner.
The ingredient is glacial acetic acid, and the adding amount is 5-15% of the mass of the organic resin.
A preparation method of a standard sample of imperfect wheat grains comprises the following steps:
(1) collecting a standard sample of imperfect wheat grains: the collection method is adopted for worm eaten grains, diseased speckles and damaged grains, and the collection standard is as follows:
worm eroding grains: granules damaged by worm decay and damaging the embryo or endosperm;
scab particles: granules with diseased spots, damaged embryos or endosperm on the grain surface;
broken particles: flattening, crushing, damaging particles of the embryo or endosperm;
(2) preparing and screening the gemmules: selecting normal wheat with consistent size, cleaning, removing impurities, laying 2-3 layers of filter paper in a culture dish, injecting clear water until the wheat is saturated, uniformly placing the seeds on the filter paper, covering the filter paper, placing the filter paper in an artificial climate box, culturing at 18-22 ℃, observing, collecting and airing according to different germination degrees, and preparing for screening standard samples; pouring the prepared wheat germinal grain sample into a white magnetic disk for primary screening, classifying according to the wheat germinal degree, making marks one by one, preparing classified seeds for fine screening, and screening to obtain germinal grains of 3 types: the embryo seed coat is broken; the bud or the radicle breaks through the seed coat and does not exceed the length of the particle; the seed coat bulges and is separated from the embryo;
(3) preparation and screening of the mildew granules: selecting normal wheat with consistent size, cleaning, removing impurities, adding water while stirring by a spray water-coating method to make the water content of the wheat reach 14-15%, then placing into a wide-mouth bottle with a cover, placing into a 42-48 ℃ artificial climate box, observing until the grain surface is mildewed, collecting, airing, and preparing for screening standard samples; pouring the prepared wheat mildew grain samples into a white magnetic disc for primary screening, classifying according to the wheat mildew degree, making marks one by one, preparing classified grains for fine screening, and after screening, classifying the wheat mildew grains into 4 types: light mildewing, sporadic mildewing on the grain surface; moderate mildew, mildew with a grain size of about 1/2 areas; the mold is more serious, and the mold is generated in about 3/4 areas of the grain surface; severe mildew is generated, and the grain surface almost generates mildew;
(4) and (4) embedding the imperfect wheat grains collected and screened in the steps (1) to (3) by using organic resin to prepare an imperfect wheat grain standard sample.
The invention has the beneficial effects that: the imperfect wheat grain standard sample prepared by the invention comprises 5 samples of worm eaten grains, scab grains, damaged grains, mildewed grains and germinated grains, has good uniformity and stability, is easy to store, and has an effective period of more than 10 years. The standard sample of imperfect grains of wheat prepared by the invention is the first creation, the preparation of the work fills the blank of the preparation of the standard sample of imperfect grains of grains at home and abroad, and the standardization of the project inspection work of imperfect grains of grains in China has important significance.
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FIG. 1 is a technical route for developing a standard sample of imperfect wheat grains.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
FIG. 1 is a technical route for developing a standard sample of imperfect wheat grains.
EXAMPLE 1 determination of evaluation criteria
Determining the most main and common standard for judging defective wheat grains in China at present, namely GB 1351-2008 wheat, as a text standard for making reference for a standard sample of defective wheat grains in the project, wherein the standard defines 5 seed projects which are main and common to the defective wheat grains as follows:
1) wormhead kernel (infected kernel): damaged by worms, damaging the granules of the embryo or endosperm.
2) Lesion kernel (spotted kernel): the grain surface has diseased spots, damages the granules of embryo or endosperm.
Black embryo (black germ kernel): the kernel embryo is dark brown or black, damaging the granules of the embryo or endosperm.
Gibberella damaged kernel: the grains are shriveled, are white, some grains are purple or have obvious pink mildew, and black ascochyta is arranged among the grains.
3) Broken pellet (brookenel): crush, damage particles of the embryo or endosperm.
4) Sprouted kernel: particles in which the germ portion seed coat has been broken or significantly raised and separated from the embryo though the bud or radicle does not break through the seed coat, or particles in which the bud or radicle does not break through the seed coat more than the length of the particle.
5) Mold kernel (molding kernel): granules with mildewed grain surfaces.
Example 2 Collection and screening of wormhole, lesion and granule
1. Collecting and screening worm-eaten grains
The standard sample development unit, namely the crop scientific research institute of Chinese agricultural academy of sciences/cereal quality supervision, inspection and test center of agricultural rural department, undertakes multiple items such as national wheat product quality safety risk assessment item, national food product quality safety special item monitoring, regional test quality analysis and evaluation of new wheat varieties in China and parts of provinces, quality spot check of different wheat varieties, pilot test evaluation and analysis, high-yield and high-quality wheat quality evaluation research and the like, and collects 5000 parts of wheat samples in total in recent years, which covers more than 300 winter and spring wheat varieties of 14 provinces in the main wheat production area of China. In the process of developing the standard sample, the developing unit combines daily wheat quality inspection work, collects and sorts the wheat worm eaten grains in the 5000 rest samples, then places the samples in a dryer for storage at room temperature, and prepares for screening the standard sample.
The collected wheat worm-eaten grain samples are poured into a white disk for primary screening. The primary screening process is mainly based on whether wheat embryo and endosperm are damaged by worms or not, and the selected seeds are prepared for fine screening. After fine screening, the obtained wormhead grains are divided into 5 types:
1) the harmful substances are wormholes and the harmful degree is light;
2) the harmful substances are wormholes and the harmful degree is high;
3) the harmful shape is a tunnel, and the harmful degree is light;
4) the harmful shape is a tunnel, and the harmful degree is heavy;
5) the embryo is damaged by worms.
2. Collection and screening of lesion particles
The standard sample development unit, namely the crop scientific research institute of Chinese agricultural academy of sciences/cereal quality supervision, inspection and test center of agricultural rural department, undertakes multiple items such as national wheat product quality safety risk assessment item, national food product quality safety special item monitoring, regional test quality analysis and evaluation of new wheat varieties in China and parts of provinces, quality spot check of different wheat varieties, pilot test evaluation and analysis, high-yield and high-quality wheat quality evaluation research and the like, and collects 5000 parts of wheat samples in total in recent years, which covers more than 300 winter and spring wheat varieties of 14 provinces in the main wheat production area of China. In the process of developing the standard sample, the developing unit combines daily wheat quality inspection work, collects and sorts wheat scab grains (mainly black embryo grains) in the more than 5000 samples, and then stores the wheat scab grains in a dryer at room temperature to prepare for screening the standard sample.
Meanwhile, the research and development is carried out in 2012 in China, Jiangsu, Anhui, Henan and other provinces with serious wheat scab disease in China, field collection work of wheat scab disease grains is carried out, scab disease field blocks are selected, wheat scab spikes with different disease degrees are cut off, the wheat scab spikes are naturally dried and threshed in a laboratory, and the samples are placed in a dryer and stored at room temperature completely and are prepared for screening standard samples.
The collected wheat scab samples were poured into a white disk for primary screening. The primary screening process is mainly based on the fact that whether wheat grain surfaces have disease spots or not, embryo or endosperm is damaged for selection, the black embryo grains and the gibberellic disease grains are respectively marked, and classified seeds are prepared for fine screening. After fine screening, the obtained scab particles are divided into the following types:
1) black embryo granule
Black sharp particles: the embryo part and the periphery of the embryo are dark brown or black and damage the embryo, and the damage degree is divided into two conditions of light damage degree and heavy damage degree;
black speck: the surfaces of the embryo and the endosperm are dark brown or black plaques, the plaque accumulation exceeds over one half of the surface area of the seeds or exceeds over one half of the abdominal furrow, and the conditions are divided into two conditions of light damage degree and heavy damage degree.
2) Granules of gibberellic disease
The grains are wrinkled and white;
the granules are purple or have obvious pink mildew-like substances, and black ascochyta shells are arranged among the granules, so the damage degree is light;
the granules are purple or have obvious pink mildew-like substances, and black ascochyta shells are arranged among the granules, which are in the harmful degree;
the granules are purple or have obvious pink mildew-like substances, and black ascochyta shells are arranged among the granules, so the damage degree is high.
3. Collection and screening of damaged pellets
The standard sample development unit, namely the crop scientific research institute of Chinese agricultural academy of sciences/cereal quality supervision, inspection and test center of agricultural rural department, undertakes multiple items such as national wheat product quality safety risk assessment item, national food product quality safety special item monitoring, regional test quality analysis and evaluation of new wheat varieties in China and parts of provinces, quality spot check of different wheat varieties, pilot test evaluation and analysis, high-yield and high-quality wheat quality evaluation research and the like, and collects 5000 parts of wheat samples in total in recent years, which covers more than 300 winter and spring wheat varieties of 14 provinces in the main wheat production area of China. In the process of developing the standard sample, the developing unit combines daily wheat quality inspection work, collects and sorts the damaged wheat grains in the more than 5000 samples, then places the samples in a dryer for storage at room temperature, and prepares for screening the standard sample.
The collected broken wheat grain samples were poured into a white disk for primary screening. The primary screening process is mainly based on whether the damage degree of wheat grains damages embryo and endosperm. The selected seeds are prepared for fine screening. After primary and fine screening, the damaged grains are divided into 2 types:
1) granules that break and damage the embryo or endosperm;
2) crush and damage the granules of the embryo or endosperm.
EXAMPLE 3 preparation and screening of germinated kernels
According to the germination reason of wheat, selecting intact wheat, culturing under proper temperature and humidity, collecting according to a set time period, finally summarizing, and classifying according to different germination degrees.
Before the sprouting grains are produced, preparation work is firstly made, including selecting the environment, culture vessels and the like for sprouting the wheat, and then special personnel are arranged to take charge of daily management.
The specific preparation method comprises the following steps: selecting normal wheat with proper size, cleaning, removing impurities, laying 2-3 layers of filter paper in a culture dish, injecting clear water until the wheat is saturated, uniformly placing the seeds on the filter paper, covering the filter paper, placing the seeds in a phytotron, culturing at 20 ℃, observing in time, collecting and drying according to different germination degrees, and preparing for screening standard samples (tools such as the culture dish, the filter paper and the like and water and the like are all disinfected).
The prepared wheat germinal grain samples were poured into a white disk for primary screening. The primary screening process is mainly based on the wheat germination degree to classify, and make identification one by one, and prepare the classified seeds for fine screening. After screening, the obtained germinated seeds are divided into 3 types:
the embryo seed coat is broken;
the bud or the radicle breaks through the seed coat and does not exceed the length of the particle;
the seed coat bulges and separates from the embryo.
EXAMPLE 4 preparation and screening of mildewed pellets
According to the reason that the wheat has mildewed grains, intact wheat is selected, cultured under the appropriate temperature and humidity, collected according to the set time period, finally summarized, and classified according to different mildewing degrees.
Before the mildewed grains are made, firstly, preparation work is done, including selecting a wheat mildewed environment, a culture vessel and the like, and secondly, special personnel are arranged to take charge of daily management.
The specific preparation method comprises the following steps: selecting normal wheat with proper size, cleaning, removing impurities, adding water while stirring by a spray water-coating method to enable the water content of the wheat to reach 14% -15%, then putting the wheat into a wide-mouth bottle with a cover, putting the wide-mouth bottle into a 45 ℃ artificial climate box, regularly observing until the grain surface is mildewed, collecting, airing, and preparing for screening standard samples.
And pouring the prepared wheat mildewed grain sample into a white disk for primary screening. The primary screening process is mainly based on the wheat mildew degree to classify, and make identification one by one, and prepare the classified seeds for fine screening. After screening, the wheat mildews are divided into 4 types:
1) mild mildew formation: sporadic mildewing on the grain surface;
2) moderate mildew formation: the area of the grain surface is about 1/2 areas;
3) the mold is formed in the area of about 3/4 grain surfaces;
4) severe mildew formation: the grain surface almost mildewed.
Example 5 preparation of standard sample of imperfect wheat grains
The standard sample of the imperfect wheat grains is prepared by embedding decayed grains, scab grains, damaged grains, germinated grains and mildewed grains in organic resin.
The embedding operation comprises the following steps:
(1) manufacturing a mould, and uniformly spraying the bright paint on the surface of the mould; the bright paint comprises the following components in parts by weight: 60 parts of acrylic resin, 15 parts of talcum powder, 4 parts of pure acrylic emulsion and 4 parts of phenyldiisocyanate trimer;
(2) cleaning the mold and then assembling an outer mold;
(3) adding the filler into the organic resin, uniformly stirring, adding the ingredients, and uniformly stirring to prepare an embedding solution; the organic resin comprises the following components in parts by weight: 70 parts of polyethylene glycol, 25 parts of transparent urea-formaldehyde resin and 25 parts of epoxy resin; the filler is gunite powder, is prepared by crushing, grinding and sieving the gunite powder with a 450-mesh sieve, and the adding proportion is 8 percent of the mass of the organic resin; the ingredient is glacial acetic acid, and the adding amount of the glacial acetic acid is 6% of the mass of the organic resin;
(4) pouring the embedding liquid into a mold, and shaking the mold to ensure that the embedding liquid in the mold flows uniformly;
(5) putting the seeds into an embedding liquid, and removing the mold after the embedding liquid is completely solidified;
(6) and (5) grinding and polishing the product.
In this example, the standard sample of imperfect wheat grains was prepared by an organic resin embedding technique. The organic resin raw material is in a liquid state, has very good fluidity, can fully fill the surface of a sample, and can not be dissolved in water after being dried and solidified into a film; and the resin has extremely high transparency, so that the microscopic structure of the standard sample can be observed conveniently. The barite is selected as the filler, so that the excellent performances of flame retardance, aging resistance, oxidation resistance, heat resistance and the like of the sample material are improved, the filler cannot be replaced by other ores, such as dolomite, and the prepared sample material is poor in transparency, easy to crisp and fragile. The standard sample has 10 grains per subentry.
Example 6 testing of wheat imperfect grain Standard sample
1. In-bottle uniformity test
Randomly selecting 20 sets of prepared defective wheat grain standard samples, and observing whether 10 grains in each standard sample are corresponding defective grains.
TABLE 1 in-bottle uniformity test results for imperfect wheat grain standards
2. Uniformity test between bottles
Randomly selecting 20 sets of the prepared defective wheat grain standard samples, and verifying whether each sub item of the 20 sets of standard samples is corresponding defective wheat grain.
TABLE 2 results of uniformity test among imperfect wheat grain standard sample bottles
3. Stability test
The biological appearance characteristics of the seeds can not change greatly along with the time, and the seeds are embedded in the resin, so that the appearance changes caused by oxidation, mildewing, deterioration and damage of external mechanical force are avoided, the change of the storage conditions has no influence on the appearance of the standard sample, and the identification characteristics of the standard sample are stable for a long time. Meanwhile, the temperature range endured by the high-permeability epoxy resin used in the project is-50 to +180 ℃, and the temperature range of standard sample transportation and storage is met.
The stability of the standard sample of the imperfect wheat grains is verified only by observing with naked eyes or observing by using a magnifying glass and a dissecting mirror, and whether the resin is changed under different storage conditions, whether each identification characteristic of the imperfect wheat grains is changed and whether the generated change affects result identification are observed.
4. Short term stability test
The stability of the imperfect wheat grain standard sample is tested under the conditions of-20 ℃, 25 ℃, 37 ℃ and 45 ℃. The test time was 4 days and 7 days.
Randomly selecting 10 sets of prepared standard samples of the imperfect wheat grains, and observing whether the resin changes under different storage conditions, whether each identification characteristic of the imperfect wheat grains changes, and whether the generated change affects result identification. Experiments show that the resin is not cracked under the extreme condition of-20 ℃, the resin is not softened under the condition of 45 ℃, the morphological characteristics of imperfect particles in the resin are not changed, and the result identification is not influenced. Similarly, the resin and the imperfect particles in the resin were not changed after the resin was left at 25 ℃ and 37 ℃ for 4 days and 7 days. The detailed test results are shown in tables 3-10.
TABLE 3 stability test results of imperfect wheat grain standard samples left at-20 ℃ for 4 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
TABLE 4 stability test results of imperfect wheat grain standard samples left at-20 ℃ for 7 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
TABLE 5 stability test results of imperfect wheat grain standard samples left at 25 ℃ for 4 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
TABLE 6 stability test results of imperfect wheat grain standard samples left at 25 ℃ for 7 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
TABLE 7 stability test results of imperfect wheat grain standard samples left at 37 ℃ for 4 days
TABLE 8 stability test results of imperfect wheat grain standard samples left at 37 ℃ for 7 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
TABLE 9 stability test results of imperfect wheat grain standard samples left at 45 ℃ for 4 days
TABLE 10 stability test results of imperfect wheat grain standard samples left at 45 ℃ for 7 days
| Sample number | Wormhole granule | Granule for treating scab | Broken granule | Sprouting granules | Mould-producing granule |
| 1 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 2 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 3 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 4 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 5 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 6 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 7 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 8 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 9 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
| 10 | 10 granules | 10 granules | 10 granules | 10 granules | 10 granules |
5. Long term stability test
The stability of the imperfect wheat grain standard sample after being stored for 6 months at normal temperature (25 ℃) under the condition of avoiding direct sunlight is tested, the imperfect grains in the resin and the resin are not changed, and the test result is shown in a table 11, so that the stability period of the imperfect wheat grain standard sample manufactured by the project is determined to be 10 years by referring to the stability period of the imperfect soybean grain standard sample manufactured by the ministry of entry and inspection and quarantine of Liaoning province.
TABLE 11 stability test results of imperfect wheat grain standard samples left at 25 ℃ for six months
Claims (7)
1. The standard sample of the imperfect wheat grains is characterized in that the standard sample of the imperfect wheat grains is prepared by embedding decayed grains, scab grains, damaged grains, germinated grains and mildewed grains with organic resin.
2. The standard sample of imperfect wheat grains of claim 1, wherein the embedding step comprises:
(1) manufacturing a mould, and uniformly spraying the bright paint on the surface of the mould;
(2) cleaning the mold and then assembling an outer mold;
(3) adding the filler into the organic resin, uniformly stirring, adding the ingredients, and uniformly stirring to prepare an embedding solution;
(4) pouring the embedding liquid into a mold, and shaking the mold to ensure that the embedding liquid in the mold flows uniformly;
(5) putting the seeds into an embedding liquid, and removing the mold after the embedding liquid is completely solidified;
(6) and (5) grinding and polishing the product.
3. The standard sample of imperfect wheat grains as set forth in claim 2, wherein the bright paint is composed of the following components in parts by weight: 50-70 parts of acrylic resin, 10-20 parts of talcum powder, 3-5 parts of pure acrylic emulsion and 3-5 parts of phenyldiisocyanate tripolymer.
4. The standard sample of imperfect wheat grains of claim 2, wherein the organic resin is composed of the following components in parts by weight: 60-80 parts of polyethylene glycol, 20-30 parts of transparent urea-formaldehyde resin and 20-30 parts of epoxy resin.
5. The standard sample of imperfect wheat grains as set forth in claim 2, wherein the filler is a barite powder prepared by pulverizing the barite powder and sieving the pulverized powder through a 400-mesh sieve and a 500-mesh sieve, and the addition ratio is 3-12% by mass of the organic resin.
6. The standard sample of imperfect wheat grains of claim 2, wherein the ingredient is glacial acetic acid and is added in an amount of 5-15% by mass of the organic resin.
7. A preparation method of a standard sample of imperfect wheat grains is characterized by comprising the following steps:
(1) collecting a standard sample of imperfect wheat grains: the collection method is adopted for worm eaten grains, diseased speckles and damaged grains, and the collection standard is as follows:
worm eroding grains: granules damaged by worm decay and damaging the embryo or endosperm;
scab particles: granules with diseased spots, damaged embryos or endosperm on the grain surface;
broken particles: flattening, crushing, damaging particles of the embryo or endosperm;
(2) preparing and screening the gemmules: selecting normal wheat with consistent size, cleaning, removing impurities, laying 2-3 layers of filter paper in a culture dish, injecting clear water until the wheat is saturated, uniformly placing the seeds on the filter paper, covering the filter paper, placing the filter paper in an artificial climate box, culturing at 18-22 ℃, observing, collecting and airing according to different germination degrees, and preparing for screening standard samples; pouring the prepared wheat germinal grain sample into a white magnetic disk for primary screening, classifying according to the wheat germinal degree, making marks one by one, preparing classified seeds for fine screening, and screening to obtain germinal grains of 3 types: the embryo seed coat is broken; the bud or the radicle breaks through the seed coat and does not exceed the length of the particle; the seed coat bulges and is separated from the embryo;
(3) preparation and screening of the mildew granules: selecting normal wheat with consistent size, cleaning, removing impurities, adding water while stirring by a spray water-coating method to make the water content of the wheat reach 14-15%, then placing into a wide-mouth bottle with a cover, placing into a 42-48 ℃ artificial climate box, observing until the grain surface is mildewed, collecting, airing, and preparing for screening standard samples; pouring the prepared wheat mildew grain samples into a white magnetic disc for primary screening, classifying according to the wheat mildew degree, making marks one by one, preparing classified grains for fine screening, and after screening, classifying the wheat mildew grains into 4 types: light mildewing, sporadic mildewing on the grain surface; moderate mildew, mildew with a grain size of about 1/2 areas; the mold is more serious, and the mold is generated in about 3/4 areas of the grain surface; severe mildew is generated, and the grain surface almost generates mildew;
(4) and (4) embedding the imperfect wheat grains collected and screened in the steps (1) to (3) by using organic resin to prepare an imperfect wheat grain standard sample.
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