FZ/T 73065-2020Knitted garments dyed by vegetable dyes (English PDF)

9.4 Product storage 12

Appendix A (Normative Appendix) Basic information of 18 vegetable dyes 13

Appendix B (Normative Appendix) Identification of Sulfur-Containing Synthetic Dyes in Textiles 21

Appendix C (Normative Appendix) Identification of 18 vegetable dyes 23

Appendix D (informative appendix) Liquid phase-mass spectra of 18 plant dye identification pigment standards 24

Knitted garments dyed with vegetable dyes

1 Scope

This standard specifies the terms and definitions, size, requirements, test methods, sampling quantity, determination rules and Instructions for use, packaging, transportation and storage this standard applies to clothing made mainly of knitted fabrics dyed with vegetable dyes.

2 Normative references the following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.

GB/T 250 Gray Sample Card for Textile Color Fastness Test to Evaluate Discoloration GB/T 1335 (all parts) clothing size GB/T 2910 (all parts) Quantitative chemical analysis of textiles GB/T 2912.1 Determination of formaldehyde in textiles Part 1: Free and hydrolyzed GB/T 3920 Textile color fastness test color fastness to rubbing GB/T 3921-2008 Textile color fastness test color fastness to soaping GB/T 3922 Textile color fastness test Color fastness to perspiration GB/T 4802.1-2008 Determination of pilling performance of textile fabrics Part 1: Circular locus method GB/T 4856 Knitted cotton fabric packaging GB/T 5296.4 Instructions for Use of Consumer Products Part 4: Textiles and Clothing GB/T 5713 Textile color fastness test color fastness to water GB/T 6411 Knitted underwear specification size series GB/T 6682 Analytical laboratory water specifications and test methods GB/T 7573 Determination of pH value of textile water extract GB/T 8170 Numerical rounding rules and the expression and determination of limit values GB/T 8427-2008 Textile color fastness test Color fastness to artificial light. xenon arc GB/T 8629-2017 Household washing and drying procedures for textile testing GB/T 14576 Textile color fastness test light and perspiration composite color fastness GB/T 14801 Test method for weft skew and bow of woven and knitted fabrics GB/T 17592 Determination of banned azo dyes in textiles GB 18401 National Basic Safety Technical Code for Textile Products GB/T 18886-2019 Textile color fastness test color fastness to saliva GB/T.19976-2005 Determination of Bursting Strength of Textiles by Steel Ball Method GB/T 29862 Labeling of textile fiber content GB/T 31127-2014 Textile Color Fastness Test Splicing and Mutual Dyeing Fastness GB 31701 Safety Technical Specification for Infant and Children's Textile Products FZ/T 01026 Textile Quantitative Chemical Analysis Multi-component Fiber Mixture FZ/T 01057 (all parts) Textile fiber identification test method FZ/T 01095 Test method for fiber content of textile spandex products FZ/T 01101 Textile fiber content determination physical method GSB16-1523 Knitted fabric pilling sample photo GSB16-2159 Standard Depth Sample Card for Knitted Products (1/12) GSB16-2500 Knitted fabric surface defect color sample photo

3 Terms and definitions the following terms and definitions apply to this document.

Vegetable dyes

Extracted from plant roots, bark, stems, leaves, fruits, seeds, etc., which can color the fiber and have a certain fastness after dyeing.

Compound.

Vegetable dyes dyed knitted garments knittedgarmentsdyedbyvegetabledyes Knitted garments made entirely of fabrics dyed with vegetable dyes, or fabrics dyed with vegetable dyes and synthetic dyes (paint dyeing (Color) fabrics are stitched together and the former area accounts for 70% or more, or the vegetable dye dyeing area accounts for 70% or more of the total area.

clothing.

Note. Mélange products do not apply to this definition, and should be analyzed based on actual products.

Type 4

According to the provisions of GB/T 6411 or GB/T 1335 (all parts), the sizes beyond the standard range shall be based on the bin value and original it can be incremented or decremented sequentially.

5 requirements

5.1 Requirements

The requirements are divided into two aspects. characteristic index, internal quality and appearance quality. The characteristic index refers to the type of dye, and the intrinsic quality includes fiber content.

Quantity, formaldehyde content, pH value, peculiar smell, decomposable carcinogenic aromatic amine dyes, color fastness to water, color fastness to perspiration, color fastness to rubbing, soaping resistance Color fastness, light fastness, light fastness, perspiration composite color fastness, splicing mutual dye fastness, saliva color fastness, washing dimensional change rate, pilling, and Bursting strong. Appearance quality includes surface defects, size deviations, symmetrical parts size differences, sewing regulations and other indicators.

5.2 Classification requirements

5.2.1 The quality level is divided into superior product, first-class product, and qualified product.

5.2.2 Quality rating. internal quality is rated by criticism, appearance quality is rated by piece, and the combination of the two is rated at the lowest level.

5.2.3 For the internal quality indicators, the lowest test result shall be used as the basis for rating the batch of products.

5.2.4 When there are appearance quality problems of different products on the same product, the lowest rating is used; only two products are allowed on the same product.

A limit surface defect of the same level exists, and the exceeding one shall be lowered by one level.

5.3 Characteristic index requirements See Table 1.

6.2.3 pH

According to GB/T 7573 regulations.

6.2.4 Odor

According to GB 18401 regulations.

6.2.5 Decomposable carcinogenic aromatic amine dyes According to GB/T 17592 regulations.

6.2.6 Color fastness to water According to GB/T 5713 regulations.

6.2.7 Color fastness to perspiration According to GB/T 3922 regulations.

6.2.8 Color fastness to rubbing Execute according to GB/T 3920 (only for straight direction).

6.2.9 Color fastness to soaping According to GB/T 3921-2008 test method A(1) regulations.

6.2.10 Color fastness to light According to the provisions of Method 3 in GB/T 8427-2008.

6.2.11 Composite color fastness to light and perspiration According to GB/T 14576 regulations.

6.2.12 Splicing and mutual dye fastness According to the provisions of Method A in GB/T 31127-2014.Among them, if there is no suitable part on the garment that can be directly sampled, it can be used in the garment or cut samples of 40mm×100mm from the same batch of fabrics of this batch of products, and then sew the two samples along the short side to form a combined sample. Correct for the sampling of products with narrow splicing fabrics or teething on the garment, the fabrics are spliced or the teething parts are disassembled, the largest area is cut, and the two samples Stitch along the short side to form a sample test.

6.2.13 Color fastness to saliva According to GB/T 18886 regulations.

6.2.14 Washing size change rate

6.2.14.1 Measuring position Tops (including jumpsuits) are the average length of the front, back, left, and right sides of the body as the calculation basis, and the measured value of the width of the back body in the horizontal direction as the basis for calculation, as shown in Figure 1;

Pants (including bibs) are calculated based on the average of the length of the left and right trousers in the vertical direction, and the average of the left and right leg widths in the horizontal direction.

6.2.14.3 Washing and drying test According to the regulations of GB/T 8629-2017, adopt A-type standard washing machine 4N program, and expressly "hand wash only" products adopt A-type Standard washing machine 4H program. Select "Standard Detergent 3" as the detergent, and the drying program is hanging to dry.

The number of test pieces is 3 pieces (strips). The samples before and after washing should be placed in an environment with a temperature of (20±2)°C and a relative humidity of (65±4)% for more than 4 hours.

Measure again.

6.2.14.4 Calculation and presentation of results According to formula (1), calculate the vertical and horizontal washing dimensional change rate, minus sign (-) indicates size shrinkage, plus sign () indicates size elongation, Take the arithmetic average of all samples as the test result. If there are two test results of contraction and upside-down, use contraction (or upside-down) two the arithmetic mean value of each sample is used as the test result. The final result shall be rounded off according to GB/T 8170, with one decimal place.

6.2.15 Pilling

According to GB/T 4802.1-2008 E law, the rating is based on GSB16-1523 sample photos.

6.2.16 Bursting strength According to the provisions of GB/T.19976-2005, the diameter of the steel ball is (38±0.02) mm.

6.3 Appearance quality inspection

6.3.1 Appearance quality inspection conditions

6.3.1.1 Generally, the inspection shall be conducted under a light source with an illuminance not less than 600lx. If natural light sources are used indoors, natural northern light shall prevail.

6.3.1.2 During the inspection, the product should be spread flat on the inspection table with a layer of white cloth on the table, and the inspector's eyes should be at least 35cm away from the cloth.

8 Judgment rules

8.1 Batch judgment

8.1.1 Judgment of characteristic index

8.1.1.1 According to the test specified in Appendix B, if the sulfur content result is higher than 0.1%, the test is terminated, and the product characteristic index of the color category is directly determined to be inferior.

qualified.

8.1.1.2 Test according to Appendix B. If the sulfur content result is less than 0.1%, continue to test according to Appendix C. If it does not contain synthetic dye If the dye name and dye identification pigment are consistent with the label, it is judged that the product characteristic index of the color category is qualified. Otherwise, it is deemed unqualified.

Note. For plant dyes other than the 18 specified in this standard, if you want to qualify, the customer must provide a valid certificate.

8.1.2 Internal quality judgment According to the requirements of this standard, if there is a non-compliance, the batch of products is determined to be unqualified. Among them, the color fastness items are not qualified, and the color is divided Determine the batch of products as unqualified.

8.1.3 Appearance quality judgment the appearance quality is calculated based on the variety and color of the non-conforming product. Where the rate of non-conforming products is within 5.0%, the batch of products is judged to be qualified and non-conforming If the product grade rate is above 5.0%, the batch of products shall be judged as unqualified.

8.1.4 Results judgment

8.1.4.1 First, determine the characteristic index according to 8.1.1.If it is unqualified, there is no need to test other items, and directly determine the product of the color.

The product is unqualified.

8.1.4.2 Those who are qualified according to 8.1.1, and then are qualified according to 8.1.2 and 8.1.3, then the product of the color category is qualified.

8.2 Single Piece Judgment If the number of product inspections is lower than the number of samples for batch determination, only the inspected samples will be determined in accordance with the provisions in 8.1, and the inspection report it is indicated in the report.

8.3 Reinspection

8.3.1 Either party may request a re-inspection when it disagrees with the inspection result.

8.3.2 The re-inspection results shall be implemented in accordance with 8.1 and 8.2, and the judgment shall be subject to the re-inspection results.

9 Instructions for use, packaging, transportation and storage

9.1 Instructions for use

9.1.1 According to the provisions of GB/T 5296.4, of which infants and children's products are implemented in accordance with the provisions of GB/T 5296.4 and GB 31701.

9.1.2 The dyed parts of vegetable dyes should be clearly indicated in the instructions for use.

9.1.3 The name of the plant dye and the dye identification pigment should be clearly indicated in the instructions for use, such as madder (alizarin), gardenia yellow (crocetin).

9.1.4 In the instructions for use, there should be words like "light may cause the fading of plant dye fabrics" to remind consumers to use them properly.

9.1.5 For products for infants and young children, the words "not dry clean" should also be marked on the instructions for use.

9.2 Product packaging

9.2.1 According to GB/T 4856 or the agreement.

9.2.2 For infants and children's products, plastic film bags should have warnings similar to the following.

---"Please put away the packaging bags in time to avoid suffocation caused by infants (children) playing"

---"Keep away from infants (children), the plastic film will stick to the nose and mouth and suffocate people

9.3 Product transportation

Product transportation should be moisture-proof, fire-proof and pollution-proof.

9.4 Product storage

Products should be stored in a cool, ventilated, dry, clean warehouse, and moth-proof and mildew-proof.

Appendix B

(Normative appendix) Identification of sulfur-containing synthetic dyes in textiles B.1 Scope this appendix specifies the method for identifying the presence of sulfur-containing synthetic dyes in fabric dyed with vegetable dyes using elemental analyzers.

B.2 Test principles

For synthetic dyes, most of the chemical structures contain sulfur. There are three main forms of sulfur. participating in the color structure such as thiol Sulfur conjugated heterocyclic structures such as azole, thioxanthene, thiazine, and thiophene; linear sulfur in sulfur dyes; vinyl sulfone reactive groups in reactive dyes; dyes are provided Water-soluble sulfonic acid group. However, there is no sulfur element in vegetable dyes, so according to whether the dye extract of the test sample contains a certain amount of sulfur, to determine whether it contains synthetic dyes.

B.3 Reagents

Concentrated hydrochloric acid (10mL concentrated hydrochloric acid is diluted with water to 30mL to obtain 4mol/L hydrochloric acid), methanol, ethanol, chloroform, ethyl acetate Etc., all of analytical grade.

B.4 Equipment and instruments B.4.1 Reactor. a round-bottomed flask made of hard glass with a closed stopper, about 100mL.

B.4.2 Constant temperature magnetic stirrer.

B.4.3 Vacuum filter device.

B.4.4 Vacuum rotary evaporator.

B.4.5 Element analyzer, main technical indicators.

1) The instrument is equipped with multiple standard operation modes such as CHNS, CHN, CNS, CN, N, S, O, etc.

2) Injection volume. 0.03mg~10mg.

3) Measuring range C. 0~40mgabs (or 100%); H. 0~3mgabs (or 100%);

N.0~15mgabs (or 100%); S.0~6mgabs (or 100%);

O.0~6mgabs (or 100%).

4) Precision (standard sample). C, H, N, S<=0.2%; O<=0.4%.

5) Correction. Non-linear correction curve, stable for a long time.

6) Gas separation method. dynamic adsorption-program desorption principle.

7) Decomposition temperature. 1150°C.

8) Sampling method. 80-position automatic sampler.

Note. Other instruments can also be used for the determination of sulfur.

B.4.6 Chromatography column.

B.4.7 One millionth balance.

B.4.8 Vacuum drying oven.

B.5 Test procedure

B.5.1 Sample pretreatment Cut out 20g of the dyed fabric sample, and wash it with 100 times (ie bath ratio 1.100) 50°C warm water in 5 times, 5 minutes each time; then use it in 5 times 100 times (i.e. bath ratio 1.100) ethanol wash at 50°C, 5min each time; then dry, cut into small pieces of 5mm×5mm, and mix well (weigh it is a mixed kind).

B.5.2 Sample preparation B.5.2.1 Preparation of non-wool dyed fabric samples Put the above mixed sample into a 250mL round bottom flask, add 100mL methanol, 20mL 4mol/L hydrochloric acid, 80°C magnetic stirring and heating Reflux for 2h, cool to room temperature, and filter under reduced pressure to obtain the dye extract of the sample. Put it on the vacuum rotary evaporator, at 50°C±1°C Concentrated under low vacuum and spin-dried, and then dried under vacuum at 50°C for 24h to obtain a powdery solid.

Note. The above extraction conditions have been verified to be applicable. During the experiment, the extraction method can also be adjusted according to the actual situation.

B.5.2.2 Preparation of dyed fabric samples containing wool Put the above mixed sample into a 250mL round bottom flask, add 100mL methanol, 10mL 12mol/L concentrated hydrochloric acid, and magnetically stir at 80°C Heat to reflux for 2h, cool to room temperature, and filter under reduced pressure to obtain the dye extract of the sample. Put it on the vacuum rotary evaporator, at 50°C± Concentrate and spin dry at 1°C under low vacuum. Then the dye is separated by column chromatography (the adsorbent is 100-200 mesh silica gel, and the eluent is ethyl acetate and methanol, V ethyl acetate. V methanol=1.0~0.1), the specific operation is as follows.

First put a certain amount of cotton into the bottom of the column, then load 100-200 mesh silica gel and compact it (the height of silica gel is 5 times the diameter of the column), and then Add ethyl acetate solution to the silica gel surface, and the above low vacuum concentration and spin-dried sample dissolved in a small amount of methanol and then added to the column (add it should be noted that the silicone surface should not be washed away). Use a dropper to add a certain amount of ethyl acetate along the inner wall of the column, and then pour the prepared eluent onto the column the ball-shaped funnel is pressurized, and the gradient elution method is adopted. First use an Erlenmeyer flask to take the solvent in the column, when the colored solution in the column reaches a certain level when the height is high, use test tube to collect. Finally, put all the dye solutions collected on a vacuum rotary evaporator at 50°C±1°C under low vacuum concentration.

Dry, and finally vacuum-dried at 50°C for 24h to obtain a powdery solid.

Note. The above extraction conditions have been verified to be applicable, and the extraction method can also be adjusted according to actual conditions during the experiment. In addition, the column chromatography eluents ethyl acetate and methanol the ratio can be adjusted accordingly according to the polarity of the dye.

B.5.3 Test

Accurately weigh 5mg of the powdered solid for elemental analysis and measure its sulfur content.

B.6 Determination of sulfur-containing synthetic dyes If the sulfur content exceeds 0.1%, it is determined that the dyed fabric contains synthetic dyes.

Appendix C

(Normative appendix) Identification of 18 kinds of vegetable dyes C.1 Principle as shown in Appendix A, 18 vegetable dyes have their own dye types, dye recognition pigments and recognition structures. Integrate with Appendix D Atlas, 18 kinds of plant dyes were identified by comparing the retention time of the sample and the standard sample liquid spectrum and the mass-to-nucleus ratio in the mass spectrum.

C.2 Reagents and instruments Methanol, concentrated hydrochloric acid (10mL of concentrated hydrochloric acid is diluted with water to 30mL to obtain 4mol/L hydrochloric acid), reactor (with a closed block, approximately 100mL round bottom flask made of hard glass), vacuum filtration device, vacuum rotary evaporator, liquid-mass spectrometer (with diode Array detector and XCT type ion trap mass detector) etc.

C.3 Test process

C.3.1 Accurately pipette an appropriate amount (about 1.0 mL) of methanol or other suitable solvents into the round bottom flask containing the powdered solid in Appendix B Medium, mix well and let stand.

C.3.2 According to the dye type and identification pigment indicated in the instructions for use, select the appropriate identification pigment standard sample working solution (Appendix D.1.1).

C.3.3 Take an appropriate amount of sample and standard sample into the chromatograph, and use the analysis conditions of the corresponding standard sample in Appendix D for testing. If so the instructions clearly indicate that there are two or more identification pigments, and the sample and the standard sample of each identification pigment should be injected into the chromatograph respectively, in turn test.

Note. Because the liquid-mass spectrogram test results depend on the instrument parameters used, it is impossible for Appendix D to give the general parameters of chromatographic analysis, but the operation in Appendix D is used.

The working conditions proved to be suitable for the test. In the actual test, the instrument parameters can be adjusted according to the instrument used.

C.4 Judgment

C.4.1 If there are obvious peaks in the liquid phase spectrum of the sample, and the retention time and mass-nucleus ratio are not in the liquid phase-mass spectrometry spectrum provided in Appendix D.

Inside the enclosure, it is considered that the fabric contains synthetic dyes or vegetable dyes other than those specified in this standard.

C.4.2 If the peak retention time and mass-nucleus ratio of the sample are consistent with the selected standard sample, and combined with Appendix A Table 1, it is considered that the fabric contains the standard sample identifies the vegetable dye corresponding to the pigment.

Appendix D

(Informative appendix) Liquid phase-mass spectra of 18 vegetable dye identification pigment standards D.1 Test conditions D.1.1 Reagents D.1.1.1 The solvent used in liquid chromatography is chromatographically pure, and the color standards are all analytically pure.

D.1.1.2 Grade 3 water meets the requirements of GB/T 6682.

D.1.1.3 Use methanol to prepare a 1000mg/L stock solution of 18 kinds of vegetable dye identification pigment standards.

D.1.1.4 Take 0.2mL from the standard stock solution and place it in a volumetric flask, and dilute to 10mL with methanol.

D.1.2 Instruments and parameters Liquid chromatography-mass spectrometer. equipped with diode array detector and XCT ion trap mass detector.

Note. Other types of detectors can also be used. The results of the atlas may differ from this standard. If other types of detectors are used, they can be provided in accordance with this standard Test principle and idea, test standard samples and samples under the same conditions and perform spectrum analysis.

Since the test results depend on the instrument parameters used, it is impossible to give the general parameters of chromatographic analysis. But use the following operations the conditions have been proven to be suitable for the test.

Liquid chromatography analysis conditions.

---Column. ZORBAXEclipseXDB-C184.6×150mm, 5µm;

---Mobile phase. acetonitrile (A). 0.1% formic acid aqueous solution (B) or methanol (C). water (D)/0.2% formic acid aqueous solution (E);

---Column temperature. 30°C;

---Detector. DAD (190nm~800nm);

--- Detection wavelength. see D.2 Note for each standard product detection;

---Flow rate. see D.2 Note for each standard test;

---Sampling amount. see D.2 Note for each standard product test;

Mass spectrometry analysis conditions.

---Sampling method. LC-MS;

---Ion source. ESI;

---Detection mode. positive ion or negative ion;

---Scan range (m/Z). 20~1500;

--- Ion source temperature (°C). see the note of each standard test in D.2;

---Atomizing gas flow rate (psi). 40;

---Drying gas flow rate (L/min). 10;

---Capillary voltage (V). 3500;

---Capillary outlet voltage (V). 109.7;

---Scan method. autoMS/MSn.

D.2 Liquid phase-ma...