CN107064469A - Proficiency testing sample that diisooctyl phthalate is determined in textile and preparation method thereof - Google Patents
Proficiency testing sample that diisooctyl phthalate is determined in textile and preparation method thereof Download PDFInfo
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- CN107064469A CN107064469A CN201710223463.8A CN201710223463A CN107064469A CN 107064469 A CN107064469 A CN 107064469A CN 201710223463 A CN201710223463 A CN 201710223463A CN 107064469 A CN107064469 A CN 107064469A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/36—Textiles
- G01N33/367—Fabric or woven textiles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
It is 484.9~2108.7mg/kg that the present invention, which discloses the concentration containing diisooctyl phthalate in a kind of proficiency testing sample determined for diisooctyl phthalate (DIDP) in textile, the proficiency testing sample,.The invention also discloses the preparation method of aforementioned capabilities verification sample.The present invention utilizes diisooctyl phthalate (DIDP), by simple PVC film material coating process, produce containing various concentrations diisooctyl phthalate (DIDP) textile PVC sample, the ability verification determined for phthalic acid ester in textile；Meanwhile, this ability verification sample preparation method is simple, success rate is high, can normal temperature storage, transport, uniformity and stability reach CNAS GL03《Proficiency testing sample homogeneity and estimation of stability guide》Requirement.
Description
Technical field
The present invention relates to textile inspection technical field.It is different more particularly, to phthalic acid two in a kind of textile
Proficiency testing sample that last of the ten Heavenly stems ester is determined and preparation method thereof.
Background technology
Phthalic ester plasticizer can be used as polyvinyl chloride (PVC) coating, painting in textile industry is widely used
Expect the solvent of stamp and hot pressing applique process, be also used as the carrier of dyeing.Taken a sample test according to relevant department, use coating, stamp
Outlet knitted dress 66% etc. technique contains different degrees of phthalic ester plasticizer.Research shows, some adjacent benzene
Diformic ester material belongs to typical environmental hormone, is classified as the 2nd class genotoxicity material by REACH regulations.So far,
World many countries put into effect regulation, standard and the content of phthalic acid ester are limited.China's mandatory national standards
《Infant and children's textile product technical specification of security》(GB 31701-2015)、《Ecological textile technical requirements》(GB/T
18885-2009) and《Clothes physicochemical property technical requirements》(GB/T 21295-2014) is to phthalate in textile
In 6 kinds of materials limited, limitation is 1000mg/kg, to detecting that underproof textile does not allow sale.Adjacent benzene two
The isodecyl ester (DIDP) of formic acid two is one of material of being limited the quantity as defined in 6 kinds.Therefore, diisooctyl phthalate in textile is strengthened
(DIDP) measure is for ensureing that textile is safe and healthy, and protection consumer's is healthy significant.
National standard《The measure tetrahydrofuran method of textile phthalic acid ester》(GB/T20388-2016) neighbour is defined
The assay method of phthalic acid ester, this method includes solvent extraction, and gas chromatograph-mass spectrometer (GC-MS) such as is measured at multiple operations
Step, any single stepping is improper all to influence the accuracy of testing result.Proficiency testing is evaluation experimental room and inspection body skill
One of important means of art ability, is also the weight for judging application accreditation and having obtained accredited laboratory and inspection body technical capability
Will according to one of.
The preparation of proficiency testing sample is the difficult point and core of phthalic acid ester measure ability verification in textile
Content, at present both at home and abroad still without relevant report.According to Chinese CNAS (CNAS) requirement, the ability of preparation is tested
Demonstrate,proving sample must be uniform enough, stably, and the content of phthalic acid ester disclosure satisfy that the requirement of merit rating.
Accordingly, it is desirable to provide developing a kind of satisfactory for diisooctyl phthalate (DIDP) in textile
Proficiency testing sample, has great importance for the detectability for examining and evaluating each laboratory.
The content of the invention
It is used to diisooctyl phthalate (DIDP) in textile it is an object of the present invention to provide one kind determine
Proficiency testing sample, the proficiency testing sample can normal temperature storage, transport, uniformity and stability reach CNAS-GL03《Ability
Verification sample uniformity and estimation of stability guide》Requirement.
It is another object of the present invention to provide a kind of preparation method of aforementioned capabilities verification sample, this method operation letter
Single, success rate is high.
To reach above-mentioned purpose, the present invention uses following technical proposals：
One kind is used for the proficiency testing sample that diisooctyl phthalate (DIDP) is determined in textile, and the ability is tested
It is 484.9~2108.7mg/kg to demonstrate,prove the concentration containing diisooctyl phthalate (DIDP) in sample.
Further, the proficiency testing sample is made up of pure cotton bleacher；The pure cotton bleacher is that pure cotton is woven
Plain weave bleacher or pure cotton twill bleacher, by pure cotton woven plain weave fabric or pure cotton grey twill by singing and bleaching
Processing is obtained.
It is preferred that, the fabric parameter of the pure cotton bleacher is：Breadth 183cm, 235/10cm of warp-wise, broadwise 234
Root/10cm, grammes per square metre 131g/m2。
It is used for the proficiency testing that diisooctyl phthalate (DIDP) is determined in textile the invention also discloses a kind of
The preparation method of sample, this method comprises the following steps：Select base fabric → modulation slurry → coating → compacting → drying → (painting
Layer-compacting-drying cycle 5 times) → bake → cooling → and cut out sample → sample homogeneity and stability test → definite value → preservation：
(1) base fabric is selected：Selection cloth cover is clean and tidy, the pure cotton bleacher without fault；The fabric parameter is：Breadth
183cm, 235/10cm of warp-wise, broadwise 234/10cm, grammes per square metre 131g/m2；
(2) slurry is modulated：12.5~50g diisooctyl phthalates (DIDP) are weighed, 10kg phthalic acids are added
In diethylester (non-disabling plasticizer), 15kg PVC paste resins (PVC, model P440) are added, are stirred；Then
Sequentially add 125g isocyanate crosslinkings, 125g organic tin stabilizers, 20g antioxidant CA, 20g antioxidant 1010,20g
UV resistance agent UV-327 and 20g UV resistance agent UV-531；
(3) coating：One side coating is taken, slurry is applied uniform in scrim surfaces；
(4) suppress：Suppressed with roller bearing press, make cloth smooth, slurry is further uniform；
(5) dry：Cloth is inserted into 110 DEG C of baking ovens, dried 4 hours；
(6) coating-compacting-drying repeatedly：Repeat this technique 5 times, PVC coatings is possessed certain thickness；
(7) bake：Under the conditions of 160 DEG C, drying is shaped 3.5 minutes, makes the abundant fusion plastifications of PVC, forms stable coatings；
(8) cool down：Cloth is taken out rapidly, cooled down at normal temperatures, makes coated film of the PVC formation with suitable intensity；
(9) sample is cut out：The full-page proof trimming prepared is cut into 5cm × 5cm sample (about 2g/ blocks), polyethylene is sub-packed in
In valve bag；
(10) sample homogeneity and stability test：According to CNAS-GL03《Proficiency testing sample homogeneity and stability are commented
Valency guide》Carry out uniformity, stability test：
1) uniformity testing
10 are randomly selected from the sample dispensed, according to national standard《The measure four of textile phthalic acid ester
Hydrogen furans method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, using single-factor side
Poor analytic approach is counted to test result, and F=3.02 is checked in by F distribution tables, such as by the calculated F of single-factor variance method
Value is less than F0.05(9,10), i.e. F<3.02, show that there was no significant difference between sample, i.e., sample is uniform；
2) stability test
Proficiency testing is presented under laboratory granting sample of respectively participating in the experiment, current traffic condition soon using common, domestic, international
Proficiency testing sample be substantially under normal temperature and transport, the internal transportation time generally requires 2-7 days, and the international transport time typically needs
Take 7-10 days；Therefore humiture environment under the conditions of simulation express delivery, randomly selects 10 parts of samples after room temperature is placed 30 days, according to state
Family's standard《The measure tetrahydrofuran method of textile phthalic acid ester》(GB/T20388-2016) method is detected as defined in,
Each sample retest 2 times, identical when the condition such as tester, instrument is with uniformity test；It will be tied obtained by uniformity testing
Fruit is cooked t inspections to the front and rear acquired results of test twice, analyzes the stabilization of sample as the first time determination data of stability test
Property；
(11) definite value：Using the average value of uniformity testing as proficiency testing sample indicated value, by the population mean
Standard deviation limited as control, be used as waning limit and action to limit 3 times of standard deviation value；
(12) preserve：Normal temperature, drying, preserve at lucifuge.
Beneficial effects of the present invention are as follows：
The present invention by simple PVC film material coating process, is produced and contained using diisooctyl phthalate (DIDP)
There is various concentrations diisooctyl phthalate (DIDP) textile PVC sample, determined for phthalic acid ester in textile
Ability verification；Meanwhile, this ability verification sample preparation method is simple, success rate is high, can normal temperature storage, transport, uniformly
Property and stability reach CNAS-GL03《Proficiency testing sample homogeneity and estimation of stability guide》Requirement.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
The low concentration proficiency testing sample of embodiment 1：Diisooctyl phthalate (DIDP) concentration is about 509.2mg/kg
One kind is used for the preparation method of the proficiency testing sample that diisooctyl phthalate (DIDP) is determined in textile,
This method comprises the following steps：
(1) base fabric is selected：Selection cloth cover is clean and tidy, the pure cotton woven plain weave bleacher without fault, and fabric parameter is：Breadth
183cm, 235/10cm of warp-wise, broadwise 234/10cm, grammes per square metre 131g/m2。
(2) slurry is modulated：12.5g diisooctyl phthalates (DIDP) are weighed, 10kg phthalic acid diethyls are added
In ester (non-disabling plasticizer), 15kg PVC paste resins (PVC, model P440) are added, are stirred；Then successively
Add 125g isocyanate crosslinkings, 125g organic tin stabilizers, 20g antioxidant CA, 20g antioxidant 1010, the anti-purples of 20g
Outer dose of UV-327 and 20g UV resistance agent UV-531.
(3) coating：One side coating is taken, slurry is coated in scrim surfaces, makes it as uniform as possible.
(4) suppress：Suppressed with roller bearing press, make cloth smooth, slurry is further uniform.
(5) dry：Cloth is inserted into 110 DEG C of baking ovens, dried 4 hours.
(6) coating-compacting-drying repeatedly：Repeat this technique 5 times, PVC coatings is possessed certain thickness.
(7) bake：Under the conditions of 160 DEG C, drying is shaped 3.5 minutes, makes the abundant fusion plastifications of PVC, forms stable coatings.
(8) cool down：Cloth is taken out rapidly, cooled down at normal temperatures, makes coated film of the PVC formation with suitable intensity.
(9) sample is cut out：The full-page proof trimming prepared is cut into 5cm × 5cm sample (about 2g/ blocks), polyethylene is sub-packed in
In valve bag；
(10) sample homogeneity and stability test：According to CNAS-GL03《Proficiency testing sample homogeneity and stability are commented
Valency guide》Carry out uniformity, stability test.
1) uniformity testing
10 are randomly selected from the sample dispensed, according to national standard《The measure four of textile phthalic acid ester
Hydrogen furans method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, test and analysis knot
Fruit is shown in Table 1：Test result is counted using one-factor analysis of variance method, it is small through the calculated F values of single-factor variance method
In F0.05(9,10), i.e. F<3.02, show that there was no significant difference between sample, i.e., sample is uniform.
2) stability test：
10 parts of samples are randomly selected after room temperature is placed 30 days, according to national standard《The survey of textile phthalic acid ester
Determine tetrahydrofuran method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, tester,
It is identical when the conditions such as instrument are with uniformity test.The first time of uniformity testing acquired results as stability test is determined into number
According to doing t inspections to the front and rear acquired results of test twice, as a result show t values less than the t critical values under 0.05 significance, table
It is bright transmission with preserve during, the change of sample can be ignored, i.e., sample is sufficiently stable.Stability test and variance analysis
It the results are shown in Table 2.
The sample homogeneity of table 1 (DIDP) inspection data summary sheet
The sample stability of table 2 (DIDP) inspection data summary sheet
(11) definite value：Using the average value of uniformity testing as proficiency testing sample indicated value, by the population mean
Standard deviation limited as control, be used as waning limit and action to limit 3 times of standard deviation value；
(12) preserve：Normal temperature, drying, preserve at lucifuge.
Proved by sample homogeneity and stability test in 30 days, the textile obtained by preparation method of the present invention
The proficiency testing sample that middle diisooctyl phthalate (DIDP) determines, DIDP concentration is (509.2 ± 24.3) mg/kg,
It disclosure satisfy that CNAS-GL03《Proficiency testing sample homogeneity and estimation of stability guide》Requirement, its uniformity and stability
All get well enough and the appearance of outlier will not be caused.
The intermediate concentration proficiency testing sample of embodiment 2：Diisooctyl phthalate (DIDP) concentration is about 1537.2mg/
kg
One kind is used for the preparation method of the proficiency testing sample that diisooctyl phthalate (DIDP) is determined in textile,
This method comprises the following steps：
(1) base fabric is selected：Selection cloth cover is clean and tidy, the pure cotton woven plain weave bleacher without fault, and fabric parameter is：Breadth
183cm, 235/10cm of warp-wise, broadwise 234/10cm, grammes per square metre 131g/m2。
(2) slurry is modulated：40g diisooctyl phthalates (DIDP) are weighed, 10kg diethyl phthalates are added
In (non-disabling plasticizer), 15kg PVC paste resins (PVC, model P440) are added, are stirred；Then add successively
Enter 125g isocyanate crosslinkings, 125g organic tin stabilizers, 20g antioxidant CA, 20g antioxidant 1010,20g UV resistance
Agent UV-327 and 20g UV resistance agent UV-531.
(3) coating：One side coating is taken, slurry is coated in scrim surfaces, makes it as uniform as possible.
(4) suppress：Suppressed with roller bearing press, make cloth smooth, slurry is further uniform.
(5) dry：Cloth is inserted into 110 DEG C of baking ovens, dried 4 hours.
(6) coating-compacting-drying repeatedly：Repeat this technique 5 times, PVC coatings is possessed certain thickness.
(7) bake：Under the conditions of 160 DEG C, drying is shaped 3.5 minutes, makes the abundant fusion plastifications of PVC, forms stable coatings.
(8) cool down：Cloth is taken out rapidly, cooled down at normal temperatures, makes coated film of the PVC formation with suitable intensity.
(9) sample is cut out to preserve：The full-page proof trimming prepared is cut into 5cm × 5cm sample (about 2g/ blocks), is sub-packed in poly-
In ethene valve bag, normal temperature, drying, preserve at lucifuge；
(10) sample homogeneity and stability test：According to CNAS-GL03《Proficiency testing sample homogeneity and stability are commented
Valency guide》Carry out uniformity, stability test.
1) uniformity testing
10 are randomly selected from the sample dispensed, according to national standard《The measure four of textile phthalic acid ester
Hydrogen furans method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, test and analysis knot
Fruit is shown in Table 3：Test result is counted using one-factor analysis of variance method, it is small through the calculated F values of single-factor variance method
In F0.05(9,10), i.e. F<3.02, show that there was no significant difference between sample, i.e., sample is uniform.
2) stability test：
10 parts of samples are randomly selected after room temperature is placed 30 days, according to national standard《The survey of textile phthalic acid ester
Determine tetrahydrofuran method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, tester,
It is identical when the conditions such as instrument are with uniformity test.The first time of uniformity testing acquired results as stability test is determined into number
According to doing t inspections to the front and rear acquired results of test twice, as a result show t values less than the t critical values under 0.05 significance, table
It is bright transmission with preserve during, the change of sample can be ignored, i.e., sample is sufficiently stable.Stability test and variance analysis
It the results are shown in Table 4.
The sample homogeneity of table 3 (DIDP) inspection data summary sheet
The sample stability of table 4 (DIDP) inspection data summary sheet
(11) definite value：Using the average value of uniformity testing as proficiency testing sample indicated value, by the population mean
Standard deviation limited as control, be used as waning limit and action to limit 3 times of standard deviation value；
(12) preserve：Normal temperature, drying, preserve at lucifuge.
Proved by sample homogeneity and stability test in 30 days, the textile obtained by preparation method of the present invention
The proficiency testing sample that middle diisooctyl phthalate (DIDP) determines, DIDP concentration is (1537.2 ± 48.0) mg/kg,
It disclosure satisfy that CNAS-GL03《Proficiency testing sample homogeneity and estimation of stability guide》Requirement, its uniformity and stability
All get well enough and the appearance of outlier will not be caused.
The high concentration proficiency testing sample of embodiment 3：Diisooctyl phthalate (DIDP) concentration is about 2054.7mg/kg
One kind is used for the preparation method of the proficiency testing sample that diisooctyl phthalate (DIDP) is determined in textile,
This method comprises the following steps：
(1) base fabric is selected：Selection cloth cover is clean and tidy, the pure cotton woven plain weave bleacher without fault, and fabric parameter is：Breadth
183cm, 235/10cm of warp-wise, broadwise 234/10cm, grammes per square metre 131g/m2。
(2) slurry is modulated：50g diisooctyl phthalates (DIDP) are weighed, 10kg diethyl phthalates are added
In (non-disabling plasticizer), 15kg PVC paste resins (PVC, model P440) are added, are stirred；Then add successively
Enter 125g isocyanate crosslinkings, 125g organic tin stabilizers, 20g antioxidant CA, 20g antioxidant 1010,20g UV resistance
Agent UV-327 and 20g UV resistance agent UV-531.
(3) coating：One side coating is taken, slurry is coated in scrim surfaces, makes it as uniform as possible.
(4) suppress：Suppressed with roller bearing press, make cloth smooth, slurry is further uniform.
(5) dry：Cloth is inserted into 110 DEG C of baking ovens, dried 4 hours.
(6) coating-compacting-drying repeatedly：Repeat this technique 5 times, PVC coatings is possessed certain thickness.
(7) bake：Under the conditions of 160 DEG C, drying is shaped 3.5 minutes, makes the abundant fusion plastifications of PVC, forms stable coatings.
(8) cool down：Cloth is taken out rapidly, cooled down at normal temperatures, makes coated film of the PVC formation with suitable intensity.
(9) sample is cut out to preserve：The full-page proof trimming prepared is cut into 5cm × 5cm sample (about 2g/ blocks), is sub-packed in poly-
In ethene valve bag, normal temperature, drying, preserve at lucifuge；
(10) sample homogeneity and stability test：According to CNAS-GL03《Proficiency testing sample homogeneity and stability are commented
Valency guide》Carry out uniformity, stability test.
1) uniformity testing
10 are randomly selected from the sample dispensed, according to national standard《The measure four of textile phthalic acid ester
Hydrogen furans method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, test and analysis knot
Fruit is shown in Table 5：Test result is counted using one-factor analysis of variance method, it is small through the calculated F values of single-factor variance method
In F0.05(9,10), i.e. F<3.02, show that there was no significant difference between sample, i.e., sample is uniform.
2) stability test
10 parts of samples are randomly selected after room temperature is placed 30 days, according to national standard《The survey of textile phthalic acid ester
Determine tetrahydrofuran method》(GB/T20388-2016) method is detected as defined in, each sample retest 2 times, tester,
It is identical when the conditions such as instrument are with uniformity test.The first time of uniformity testing acquired results as stability test is determined into number
According to doing t inspections to the front and rear acquired results of test twice, as a result show t values less than the t critical values under 0.05 significance, table
It is bright transmission with preserve during, the change of sample can be ignored, i.e., sample is sufficiently stable.Stability test and variance analysis
It the results are shown in Table 6.
The sample homogeneity of table 5 (DIDP) inspection data summary sheet
The sample stability of table 6 (DIDP) inspection data summary sheet
(11) definite value：Using the average value of uniformity testing as proficiency testing sample indicated value, by the population mean
Standard deviation limited as control, be used as waning limit and action to limit 3 times of standard deviation value；
(12) preserve：Normal temperature, drying, preserve at lucifuge.
Proved by sample homogeneity and stability test in 30 days, the textile obtained by preparation method of the present invention
The proficiency testing sample that middle diisooctyl phthalate (DIDP) determines, DIDP concentration is (2054.7 ± 54.0) mg/kg,
It disclosure satisfy that CNAS-GL03《Proficiency testing sample homogeneity and estimation of stability guide》Requirement, its uniformity and stability
All get well enough and the appearance of outlier will not be caused.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (5)
1. a kind of be used for the proficiency testing sample that diisooctyl phthalate is determined in textile, it is characterised in that：The energy
The concentration containing diisooctyl phthalate is 484.9~2108.7mg/kg in power verification sample.
2. proficiency testing sample according to claim 1, it is characterised in that：The proficiency testing sample bleaches base by pure cotton
Cloth is made.
3. proficiency testing sample according to claim 2, it is characterised in that：The pure cotton bleacher is that pure cotton is woven flat
Line bleacher or pure cotton twill bleacher, by pure cotton woven plain weave fabric or pure cotton grey twill by singing and bleaching
Reason is obtained.
4. the proficiency testing sample according to Claims 2 or 3, it is characterised in that：The fabric ginseng of the pure cotton bleacher
Number is：Breadth 183cm, 235/10cm of warp-wise, broadwise 234/10cm, grammes per square metre 131g/m2。
5. a kind of ability determined as described in claim 1-4 is any for diisooctyl phthalate in textile for preparing is tested
The method for demonstrate,proving sample, it is characterised in that comprise the following steps：
(1) base fabric is selected：Selection cloth cover is clean and tidy, the pure cotton bleacher without fault；
(2) slurry is modulated：12.5~50g diisooctyl phthalates are weighed, are added in 10kg diethyl phthalates, then
15kg PVC paste resins are added, are stirred；Then 125g isocyanate crosslinkings, 125g Organotin Stabilizeds are sequentially added
Agent, 20g antioxidant CA, 20g antioxidant 1010,20g UV resistance agent UV-327 and 20g UV resistance agent UV-531；
(3) coating：One side coating is taken, slurry is applied uniform in scrim surfaces；
(4) suppress：Suppressed with roller bearing press；
(5) dry：Cloth is inserted into 110 DEG C of baking ovens, dried 4 hours；
(6) coating-compacting-drying repeatedly：Repeat this technique 5 times；
(7) bake：Under the conditions of 160 DEG C, drying is shaped 3.5 minutes；
(8) cool down：Cloth is taken out rapidly, cooled down；
(9) sample is cut out：The full-page proof trimming prepared is cut into 5cm × 5cm sample, dispensed；
(10) sample homogeneity and stability test：According to CNAS-GL03《Proficiency testing sample homogeneity and estimation of stability refer to
South》Carry out uniformity, stability test：
(11) definite value：Using the average value of uniformity testing as proficiency testing sample indicated value, by the mark of the population mean
Quasi- deviation is limited as control, and 3 times of values of the standard deviation are limited as waning limit and action.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107462450A (en) * | 2017-08-22 | 2017-12-12 | 中纺协检验（泉州）技术服务有限公司 | A kind of production method of standard specimen textile |
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