Some standard content:
1cS 83.180
National Standard of the People's Republic of China
GB 19340--2003
Adhesives for footwear and base and bag
Adhesives for footwear and base and bag2003-10-09Promulgated
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
2004-06-01Implementation
Chapter 3, Article 4 of this standard is a mandatory clause. The rest are recommended clauses. The appendices of this standard, Appendix A, Appendix B and Appendix (:) are normative appendices. The standard was proposed by the China Petroleum and Chemical Industry Association and was issued by the National Adhesive Standardization Technical Committee. 11-TTKAONT KAca-
GB 19340—2003
The responsible drafting units of this standard are: Shanghai Rubber Products Research Institute, Chemical Industry Adhesive Quality Supervision and Inspection Center, China Adhesive Industry Association.
Participating drafting units of this standard are: Nanhai Nanguang Chemical Packaging Co., Ltd., Nanhai Bali Chemical Products Co., Ltd., Zhenjiang Jinbao Adhesive Co., Ltd.
Drafters of this standard: Gong Dinglin, Jin Weixing, Shen Yihua, Gong Meifen, Ju Wenhan, Li Xianquan, Jiao Zhuoni This standard cannot replace HG/T2493—1993 "Chloroprene Rubber Adhesive for Shoes" This standard is entrusted to the National Adhesive Standardization Technical Committee for interpretation. 1 Scope
Adhesive for shoes and bags
This standard specifies the bonding performance, harmful substance limits and test methods of adhesives for shoes and bags. This standard is applicable to adhesives for shoes and bags, GB 19340-2003
This standard does not include all safety issues related to users. Therefore, users are responsible for establishing relevant safety and health clauses and determining the specified scope of use before use to meet relevant national regulations (such as the concentration of harmful substances in the workshop air, etc.). 2 Normative reference documents
The clauses in the following documents are cited in this standard and become the clauses of this standard. They are referenced documents with a date of month. All subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, Parties that reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. They are undated references, and their latest versions apply to this standard. (: B/T32 Determination of the bond strength of vulcanized rubber or thermoplastic rubber to fabric (itTSO) 3F) B/T7[24 Test method for tensile shear strength of adhesives (metal to metal) c9[S()4587) (GB18583 Limitation of substances in adhesives for interior decoration and furnishing materials 1IG/12815 Test method for heat resistance of light-use adhesives H (F/T 3075 Regulations for packaging, marking, transportation and storage of adhesive products 3 Technical requirements
3.1 The adhesive properties of shoe adhesives used for bonding shoe soles to soles and shoe soles shall comply with the requirements of Table 1. Table 1 Adhesive properties of shoe adhesives
Initial adhesion/(N,mm)
Color strength Nm:)
Heat aging resistance: N/mto
Shear strength MPa
Variation/mm
These adhesive properties requirements only apply to shoes worn under normal conditions. For special footwear that needs to withstand additional loads and/or other external conditions, such as safety shoes, work shoes or sports shoes, additional tests shall be carried out. 3.2 Recommended test materials Www.bzxZ.net
3.2.1 The test materials and bonding processes can be specified by the manufacturer and the user. The bonding properties shall not be lower than the index values of the corresponding items in Table 1. The test results obtained from the test materials for this adhesive cannot be applied to similar materials without conditions. This adhesive must be used to test the shoe materials actually used to ensure that they meet the requirements of the above table. The following test materials are recommended: a) Recommended test material Leather 1: Sole leather: b) Recommended test material Leather 2: Sole leather. Plant-based: Recommended test material SBR 1: Tetraphenyl rubber. Shore A hardness 95td) Recommended test material S1K2 Polyethylene rubber, Shore A hardness 70: e) Recommended test material NBR: Polyethylene rubber. Shore A hardness: GB 19340—2003 f) Recommended test material SISR: Thermoplastic rubber, Shore A hardness 60 h) Recommended test material PVC: Soft vinyl chloride, Shore A hardness 70-TTKAONIKACa The performance of the recommended test materials should not affect the bonding performance test of the adhesive. The hardness given as a characteristic is only used to distinguish between different materials. 3.2.2 Recommended test materials The following material combinations are used to prepare the test specimens: Leather 1/SBR1
Leather 1/Leather 2
SBRI/SBR1
SBR2/SBR2
NBR/NBR
SBSR/SBSR
PVC/PVC
Fur 1/SBR! The sample is used to judge the bonding performance of adhesive to the most commonly used interlayer leather in the shoe industry. It is used to judge the adhesive with higher body strength than leather 1. The recommended test materials are leather 2. SBR1. SBR2. NBR, SBSR and PVC. Two identical recommended test materials are used for testing. Leather 1/SBR1 samples (such as polychloroprene adhesive) or leather 1/PVC samples (such as polyurethane adhesive) can be used for end-to-end peeling test (50℃2℃)
3.3 Except for the instrument used for process positioning, the peel strength of the adhesive for luggage should not be less than 2.0N/mm. The test materials and bonding process can be specified by the manufacturer or the user. The characteristic peel strength value cannot be less than 2.N/ml. 3.4 Requirements for the limit of harmful substances in adhesives The limit of harmful substances in adhesives for shoes and bags shall comply with the provisions of Table 2. 2 Items for the limit of harmful substances in adhesives for shoes and bags Free isocyanate n-isocyanate n-isocyanate difluoroethane 1,2-ethyl chloride 1,1,2-dichloroethane Vinyl chloride Total volatile organic matter Substituted hydrocarbons Polyurethane adhesive test item 4 Test method 4.1 Adhesive materials and their treatment and sample preparation 4.1.1 Adhesive materials and surface treatment 20 kg/kg 10.0 g/kg
15Cg/kg
50. 0 g/kg
The test material and surface treatment to be bonded shall be specified by the manufacturer and the user. If not specified, proceed according to Appendix A. 4.1.2 Preparation of test specimens
4.1.2.1 Shape and size of test specimens and number of test specimens4.1.2.1.1 Initial adhesion, peel strength, heat aging resistance and coiling test specimens GB 19340--2003
The test piece is 100mm.1.2mm long and 30mm/0.5mm wide. Two test pieces are placed on the platform. The bonding length is 60mm±2mm4.1.2.1.2 Shear strength test specimen
The test piece is 80 mm±2mm long and 20 mm±0.2 mm wide. Two test pieces are overlapped and the overlap length is 10mm mm±0.2mm4.1.2.1.3 Number of samples
The number of samples shall be at least 3; the arbitration test shall be no less than 5. 4.1.3 Sample bonding process
The sample bonding process such as adhesive ratio, glue coating amount, glue coating number, air-drying time, curing degree, pressure, pressurization time, etc. shall be specified by the manufacturer and the user. If not specified, follow Appendix A. 4.2 Initial bonding
After the sample is prepared, let it stand for 2 minutes and conduct a peel test in accordance with GB/T532. The separation speed of the sample holder is 100mm/min±10 mm/min.
4.3 Peel strength
After the sample is prepared, at a temperature of 23°%±2% and a relative filtration degree of 50+5, conduct a separation test in accordance with GT532. The separation speed of the sample holder is 100 mm/min±0mnm/min. 4.4 Heat aging resistance
After the sample is prepared, it is placed at a temperature of 23℃+2℃ and a relative humidity of 50%=5% for 5 days. Then it is placed at a temperature of 50℃±2℃ for 5 days. According to the provisions of 6B/T532, the separation test is carried out. The separation speed of the sample holder is 100mnu/min±10mm/min4.5 Shear strength
After the sample is prepared, it is placed at a temperature of 23℃! 2℃ and a relative humidity of 50%±5 for 5 days. According to the provisions of GB/F7124, the shear test is carried out: the separation speed of the sample holder is 25m/min±2mm/tmin. 4.6 Degeneration
After the sample is prepared, it is placed at a temperature of 23℃.+2℃:, relative humidity 50% ± 5% after standing for 5 days, according to HG/T2815. Test temperature is 50℃±2℃, the total mass of the loading base and hook is 1.5kg. Test time is 10min. 4.7 Determination of methyl ether content is carried out according to GB18583. 4.8 Determination of toluene and methylbenzene content is carried out according to GB 18583. 4.9 The determination of free toluene monoisocyanate content shall be carried out in accordance with the provisions of GB18583. 4.10 The determination of n-hexane content shall be carried out in accordance with the provisions of Appendix B of this standard. 4.11 The determination of chloroethane, 1,2-dichloroethane, 1,1,2-triethane and ethylene fluoride content shall be carried out in accordance with the provisions of the appendix of this standard. 4.12 The determination of total volatile organic matter content shall be carried out in accordance with the provisions of GB18583. 5 Inspection rules
5.1 Inspection classification
Products can only be shipped after passing the inspection according to this standard, and a product certificate shall be attached. Product inspection is divided into factory inspection and type inspection. 5.1.1 Factory inspection
Factory inspection items for shoe adhesives: initial adhesion, peel strength, and heat aging resistance. The materials recommended by this standard shall be selected for the bonded materials. Factory inspection items for luggage adhesives: peel strength. 5.1.2 Type inspection
5.1.2. 1 Type inspection shall be conducted in any of the following cases: a) After normal production for 1 year, or when there are major changes in the formula or process that may affect the quality; h) When production is resumed after a suspension of more than 1 year; c) When the national quality supervision agency or the user makes a request. 5.1.2.2 Type inspection items GB 19340-2003 Type inspection items for shoe adhesives: limit of harmful substances, initial adhesion, peel strength, shear strength, heat aging resistance and degeneration. The materials to be bonded shall be the materials recommended by this standard. Type inspection items for luggage adhesives: limit of harmful substances, peel strength. 5.2 Batching and inspection Each batch of products is a batch, and the batches shall be inspected. 5.3 Multiplication of samples 5.3.1 The number of samples to be sampled shall be as specified in Table 3. Table 3 Product sampling quantity
Number of containers
65~-125
126-216
Minimum sampling number
Number of containers
217.--343
344--512
513-729
730--1 000
1 000 and above
Minimum sampling number
The samples taken are mixed to form a test mixed sample with a total volume of not less than 1.3 kα, which is divided into 3 test samples. The test samples are stored in a sealed container.
5.4 Inspection Result Determination
If there is an index value that does not meet the requirements of this certificate, take double samples to re-inspect the unqualified items. If the re-inspection still does not reach the corresponding standard value, the batch of adhesives is judged to be unqualified. 6 Marking, packaging, transportation and purchase and storage
Carry out according to the provisions of 11G/130?=. Adhesives for shoes and bags must be marked on the outer packaging with harmful substances and sand and safe and healthy use methods.
Test report
The test report shall include the following contents:
a) Name and number of this standard;
Adhesive name, production unit and batch number;
Name and model of instrument used;
Test results:
Abnormal conditions found during the test:
Inspector and test date
A.1 Scope
Appendix A
(Normative Appendix)
Adhesion performance test specimen preparation
This appendix specifies the preparation of test specimens for determining the adhesion performance of adhesives for bags and suitcases. A.2 Test materials and surface treatment
GB 19340-2003
The selection and surface treatment of the test materials to be bonded shall be specified by the manufacturer and user. If not specified, cowhide or styrene-butadiene rubber may be used. A, 2. 1 Cowhide
The cowhide is of first-class quality. The cowhide on the back of the cowhide should be polished with a grinding wheel until the leather breaks and the nap is raised. The dense test piece should be thoroughly cleaned of grinding debris. A. 2. 2 Styrene-butadiene rubber sheet
a) Rubber formula (parts by mass)
Styrene-butadiene rubber (SBR1502)
Zinc oxide
Accelerator M
Accelerator DM
Accelerator TMTD
High wear-resistant carbon black
Motor oil (No. 20)
1) Vulcanization conditions: (150 on 1) × 8i
c) Thickness of styrene-butadiene rubber sheet: (2! 0.3)tmm. Cotton cloth is lined on the back. d) After preparation, the styrene-butadiene rubber sheet is placed at room temperature for 24 h. e) Grinding and brushing of styrene-butadiene rubber sheets. A.3 Preparation of test specimens
The bonding process of test specimen preparation shall be specified by the manufacturer and the user, such as the adhesive ratio, the number of times of coating, the air-drying time, the curing temperature, the pressure, and the pressurizing time. If not specified, the following method shall be followed. If the adhesive is prepared in the use chamber, it shall be prepared according to the regulations of the adhesive manufacturer. For adhesive coating, the prepared and mixed adhesive can generally be applied to the two adhesive surfaces of the test material respectively, and brushed twice. After coating, it shall be allowed to stand for about 15 minutes. For absorbent materials, if it is required to be coated on the bonding surface multiple times, the number of times shall be indicated in the test report. After standing, the bonding surfaces shall be combined with each other. When combining, pinning and fire bubbles shall be prevented. Then roll along the longitudinal direction with a hand roller for 3~5 seconds, and then apply an average pressure of (0.4-~0.6)MP for 15 seconds. The conditions and time for placing the sample after preparation shall be in accordance with the provisions of each performance test:
GB 19340-2003
B.1 Scope
Appendix B
(Normative Appendix)
Determination of n-hexane content in adhesives for shoes and bags Gas chromatography This method specifies the method for determining the content of harmful substances n-hexane in adhesives for shoes and bags. This method is applicable to the determination of adhesives for shoes, bags and suitcases with a hexane content of less than 0.1%/kg. B.2 Principle
KAONiKAca-
After the sample is dissolved with an appropriate solvent, the diluted sample solution is directly injected into the injection device with a micro syringe. It is carried into the chromatographic column by the carrier gas and separated into corresponding fractions in the chromatographic column. The chromatogram is detected and recorded by the hydrogen flame ionization detector. The content of harmful substances in the sample solution is calculated by the external standard method.
B.3 Reagents
R, 3.1 Hexane: chromatographic grade,
B. 3.2 Ethylene glycol: analytical grade.
B.4 Instruments
Injector: 5 μm micro syringe,
Chromatograph: with ammonia flame ionization detector. Chromatographic column: capillary column (50 m×0.20 mm 0.sμm), the stationary liquid is siloxane\. B, 4.3
Recording equipment: integrator or chromatographic workstation. B. 4. 4
Measurement conditions
Vaporization chamber temperature: 200℃;
B. 4. 5. 1
Detection air temperature: 250℃,
B. 4. 5. 2
Nitrogen: purity greater than 99.999%, dehydration by silica gel, column head pressure of 70 kPa (.30℃); R, 4. 5. 3
Hydrogen: purity greater than 99.999%, dehydration by silica gel, column head pressure of 65 kPa; B. 4. 5, 4
B,4. 5. 5: dehydration by silica gel, column head pressure of 55 kPaB. 4. 5. 6
Split, split ratio is 20:1;
B. 4. 5. 7
Tail blowing: 30 ml.
B. 4. 5. 8
Programmed temperature rise
1st stage: initial temperature 30℃, holding time 30 min, heating rate 2℃/min, final temperature 60℃. 2nd stage: initial temperature 60℃, holding time 0rri, heating rate 5℃/min, final temperature 90%℃, 3rd stage: initial temperature 90℃, holding time 10min, heating rate 10℃:/min + final temperature 150℃, holding time 10minB.5 Analysis steps
Weigh 0.2~0.3 (accurate to 0.1ng) of sample and place it in a 5mL volumetric flask. Dilute to the scale with butyl acetate. Use 5L of ionizer to take 2.0 injections and measure the peak area. If the peak area of the sample is larger than the peak area of the highest concentration, use a liquid pipette to accurately transfer a small volume of the sample and dissolve it in a 50 ml container. Dilute it to the mark with nicotinic acid and shake it. Then, mix it and mix it. When some components are difficult to separate from the sensitive components, it is necessary to conduct the test under appropriate conditions for different properties.
B.6 Preparation of standard solution
B.6.1 Standard solution: about 10 g/mL
CB19340—2003
Weigh about 1 g (accurate to 0.1 mg) of n-dioxane, place it in a 300-mL volumetric flask, dilute to the mark with butyl acetate, and shake well. B.6.2 Standard solution: 500 μg/mL
Take an appropriate volume of hexane standard solution (B.6.1), place it in a 100-mL volumetric flask, dilute to the mark with butanone, and shake well to obtain a standard solution with a n-hexane concentration of 50 μg/mL. B.6.3 Preparation of series standard solutions
Pipette the volumes of standard solution (B.6.2) listed in Table B.1, place them in six 25-mL volumetric flasks, and dilute to the mark with butyl acetate.
Table B.1 Volume of series of standard solutions and volume of corresponding concentration shift
B.6.4 Determination of peak area of series of standard quenching solutions Take the concentration of n-hexane,
(pR/ml)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5 μl syringe to take 2.0 μl of standard solution and inject it. Determine the peak area. Inject three times of each standard solution and take the average value. B.6.5 Drawing of standard curve
Use the peak product A of n-hexane as the ordinate and the corresponding concentration (μg/mL) as the abscissa: the standard curve of n-hexane is obtained. B.7 Expression of results
Read the hexane concentration of the sample solution directly from the standard curve or calculate it according to the homogeneous equation. The content of n-hexane in the sample is calculated by the formula: cvf
wherein:
X is the content of n-hexane in the sample, in grams per gram (/kg); - the concentration of n-hexane in the sample solution, in micrograms per milliliter (μg/nmE); the volume of the sample solution, in milliliters (\I.); - the mass of the sample, in grams (g):
f is the dilution multiple of the sample solution.
CB 19340—2003
c.1 Scope
(Normative Appendix)
Determination of halogenated hydrocarbons in adhesives for shoes and bags by gas chromatography-gas ...
C.2 Principle
The sample is dissolved in an appropriate solvent, and the sample is injected into the sample chamber through a micro-injector. The sample is then introduced into the chromatographic column and separated into corresponding components. The chromatogram is detected and recorded using a hydrogen flame ionization detector. The content of the measured components in the sample solution is calculated using the external standard method.
C.3 Reagents
C.3.1-Methylene chloride, 1,2-difluoroethane, 1,1,2-trichloroethane, and vinyl chloride are all chromatographically pure. C.3.2 Acid esters: analytically pure
C.4 Instruments
C.4.1 Injector: 5 μl micro-injector. C.4.2 Chromatographic column with hydrogen flame ionization detector. C.4.3 Chromatographic column: capillary column (50 m×0.20 nm×0.5 um). The stationary liquid is polysiloxane. C.4.4 Recording device: integrator or chromatographic workstation. C.4.5 Determination conditions
Vaporization chamber temperature: 200°C+
C. 4. 5. 1
C, 4, 5, 2
Detection density: 250%
Nitrogen: purity greater than 99,999%, silica gel dehydration, column head pressure of 70 kPa30℃): C. 4. 5. 31
Hydrogen, purity greater than 99.999%, silica gel dehydration, column head pressure of 65 kPaC. 4. 5. 4
C. 4. 5. 5
Air: silica gel dehydration, column head pressure of 55 kPa: split, split ratio is 20:1:
C. 4. 5. 6:
Blowing: 30 ml.
C. 4. 5. 71
C. 4,5. 8 Program source
1st stage: initial temperature 30℃. Holding time 30min. Heating rate 2%℃/min, final temperature 60℃, 2nd stage: initial temperature 60%, holding time 0min. Heating rate 5℃/min, final temperature 90℃, 3rd stage: initial temperature 90%. Holding time 0min, heating rate 10~./min, final temperature 150℃. Holding time 11min.C.5 Analysis steps
Take (0.2 g~0.3% accurate to 0.1 Img) sample, microcentrifuge 0 ml. Dissolve in ethyl acetate and dilute to the mark. Shake well. [When the peaks of the measured components are difficult to separate due to other components, it is necessary to switch to this type of reagent and conduct the test under appropriate conditions. GB19340--2003
Use a 5L syringe to take 2.0μ1. Inject the sample and check its area. If the frontal area of the sample solution is larger than the peak area of the maximum concentration, use a pipette to transfer an appropriate amount of sample solution to a 50 mL volumetric flask. Dilute to the mark with ethyl acetate, shake and measure again. C.6 Preparation of standard solution
C.6.1 Standard solution: about 10 mg/mL
Weigh about 1 g (accurate to 0.1 m&) of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride respectively and place them in four 100 mL volumetric flasks, dilute to the mark with ethyl acetate, mix well, C.6.2 Standard solution; 500 μ/mL
Pipette an appropriate amount of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride standard solution respectively and place them in a 190 mL. Dilute to the mark with ethyl acetate in a volumetric flask and shake to obtain a standard solution of dimethane, 1,2-diethane, 1,1,2-diethylenetriamine and trifluoroethylene with a concentration of 500 μg/mL. C.6.3 Preparation of a series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place it in six 25 ml volumetric flasks, dilute to the mark with ethyl acetate and shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)Dilute with butyl acetate.
Table B.1 Volume of series of standard solutions and volume of corresponding concentration shift
B.6.4 Determination of peak area of series of standard quenching solution Take the concentration of n-hexane,
(pR/ml)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5 μl syringe to take 2.0 μl of standard solution and inject it. Determine the peak area. Inject three times of each standard solution and take the average value. B.6.5 Drawing of standard curve
Use the peak product A of n-hexane as the ordinate and the corresponding concentration (μl/mL) as the abscissa: the standard curve of n-hexane is obtained. B.7 Expression of results
Read the hexane concentration of the sample solution directly from the standard curve or calculate it according to the homogeneous equation. The content of n-hexane in the sample is calculated by the formula: cvf
wherein:
X is the content of n-hexane in the sample, in grams per gram (/kg); - the concentration of n-hexane in the sample solution, in micrograms per milliliter (μg/nmE); the volume of the sample solution, in milliliters (\I.); - the mass of the sample, in grams (g):
f is the dilution multiple of the sample solution.
CB 19340—2003
c.1 Scope
(Normative Appendix)
Determination of halogenated hydrocarbons in adhesives for shoes and bags by gas chromatography-gas ...
C.2 Principle
The sample is dissolved in an appropriate solvent, and the sample is injected into the sample chamber through a micro-injector. The sample is then introduced into the chromatographic column and separated into corresponding components. The chromatogram is detected and recorded using a hydrogen flame ionization detector. The content of the measured components in the sample solution is calculated using the external standard method.
C.3 Reagents
C.3.1-Methylene chloride, 1,2-difluoroethane, 1,1,2-trichloroethane, and vinyl chloride are all chromatographically pure. C.3.2 Acid esters: analytically pure
C.4 Instruments
C.4.1 Injector: 5 μl micro-injector. C.4.2 Chromatographic column with hydrogen flame ionization detector. C.4.3 Chromatographic column: capillary column (50 m×0.20 nm×0.5 um). The stationary liquid is polysiloxane. C.4.4 Recording device: integrator or chromatographic workstation. C.4.5 Determination conditions
Vaporization chamber temperature: 200°C+
C. 4. 5. 1
C, 4, 5, 2
Detection density: 250%
Nitrogen: purity greater than 99,999%, silica gel dehydration, column head pressure of 70 kPa30℃): C. 4. 5. 31
Hydrogen, purity greater than 99.999%, silica gel dehydration, column head pressure of 65 kPaC. 4. 5. 4
C. 4. 5. 5
Air: silica gel dehydration, column head pressure of 55 kPa: split, split ratio is 20:1:
C. 4. 5. 6:
Blowing: 30 ml.
C. 4. 5. 71
C. 4,5. 8 Program source
1st stage: initial temperature 30℃. Holding time 30min. Heating rate 2%℃/min, final temperature 60℃, 2nd stage: initial temperature 60%, holding time 0min. Heating rate 5℃/min, final temperature 90℃, 3rd stage: initial temperature 90%. Holding time 0min, heating rate 10~./min, final temperature 150℃. Holding time 11min.C.5 Analysis steps
Take (0.2 g~0.3% accurate to 0.1 Img) sample, microcentrifuge 0 ml. Dissolve in ethyl acetate and dilute to the mark. Shake well. [When the peaks of the measured components are difficult to separate due to other components, it is necessary to switch to this type of reagent and conduct the test under appropriate conditions. GB19340--2003
Use a 5L syringe to take 2.0μ1. Inject the sample and check its area. If the frontal area of the sample solution is larger than the peak area of the maximum concentration, use a pipette to transfer an appropriate amount of sample solution to a 50 mL volumetric flask. Dilute to the mark with ethyl acetate, shake and measure again. C.6 Preparation of standard solution
C.6.1 Standard solution: about 10 mg/mL
Weigh about 1 g (accurate to 0.1 m&) of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride respectively and place them in four 100 mL volumetric flasks, dilute to the mark with ethyl acetate, mix well, C.6.2 Standard solution; 500 μ/mL
Pipette an appropriate amount of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride standard solution respectively and place them in a 190 mL. Dilute to the mark with ethyl acetate in a volumetric flask and shake to obtain a standard solution of dimethane, 1,2-diethane, 1,1,2-diethylenetriamine and trifluoroethylene with a concentration of 500 μg/mL. C.6.3 Preparation of a series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place it in six 25 ml volumetric flasks, dilute to the mark with ethyl acetate and shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)Dilute with butyl acetate.
Table B.1 Volume of series of standard solutions and volume of corresponding concentration shift
B.6.4 Determination of peak area of series of standard quenching solution Take the concentration of n-hexane,
(pR/ml)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5 μl syringe to take 2.0 μl of standard solution and inject it. Determine the peak area. Inject three times of each standard solution and take the average value. B.6.5 Drawing of standard curve
Use the peak product A of n-hexane as the ordinate and the corresponding concentration (μl/mL) as the abscissa: the standard curve of n-hexane is obtained. B.7 Expression of results
Read the hexane concentration of the sample solution directly from the standard curve or calculate it according to the homogeneous equation. The content of n-hexane in the sample is calculated by the formula: cvf
wherein:
X is the content of n-hexane in the sample, in grams per gram (/kg); - the concentration of n-hexane in the sample solution, in micrograms per milliliter (μg/nmE); the volume of the sample solution, in milliliters (\I.); - the mass of the sample, in grams (g):
f is the dilution multiple of the sample solution.
CB 19340—2003
c.1 Scope
(Normative Appendix)
Determination of halogenated hydrocarbons in adhesives for shoes and bags by gas chromatography-gas ...
C.2 Principle
The sample is dissolved in an appropriate solvent, and the sample is injected into the sample chamber through a micro-injector. The sample is then introduced into the chromatographic column and separated into corresponding components. The chromatogram is detected and recorded using a hydrogen flame ionization detector. The content of the measured components in the sample solution is calculated using the external standard method.
C.3 Reagents
C.3.1-Methylene chloride, 1,2-difluoroethane, 1,1,2-trichloroethane, and vinyl chloride are all chromatographically pure. C.3.2 Acid esters: analytically pure
C.4 Instruments
C.4.1 Injector: 5 μl micro-injector. C.4.2 Chromatographic column with hydrogen flame ionization detector. C.4.3 Chromatographic column: capillary column (50 m×0.20 nm×0.5 um). The stationary liquid is polysiloxane. C.4.4 Recording device: integrator or chromatographic workstation. C.4.5 Determination conditions
Vaporization chamber temperature: 200°C+
C. 4. 5. 1
C, 4, 5, 2
Detection density: 250%
Nitrogen: purity greater than 99,999%, silica gel dehydration, column head pressure of 70 kPa30℃): C. 4. 5. 31
Hydrogen, purity greater than 99.999%, silica gel dehydration, column head pressure of 65 kPaC. 4. 5. 4
C. 4. 5. 5
Air: silica gel dehydration, column head pressure of 55 kPa: split, split ratio is 20:1:
C. 4. 5. 6:
Blowing: 30 ml.
C. 4. 5. 71
C. 4,5. 8 Program source
1st stage: initial temperature 30℃. Holding time 30min. Heating rate 2%℃/min, final temperature 60℃, 2nd stage: initial temperature 60%, holding time 0min. Heating rate 5℃/min, final temperature 90℃, 3rd stage: initial temperature 90%. Holding time 0min, heating rate 10~./min, final temperature 150℃. Holding time 11min.C.5 Analysis steps
Take (0.2 g~0.3% accurate to 0.1 Img) sample, microcentrifuge 0 ml. Dissolve in ethyl acetate and dilute to the mark. Shake well. [When the peaks of the measured components are difficult to separate due to other components, it is necessary to switch to this type of reagent and conduct the test under appropriate conditions. GB19340--2003
Use a 5L syringe to take 2.0μ1. Inject the sample and check its area. If the frontal area of the sample solution is larger than the peak area of the maximum concentration, use a pipette to transfer an appropriate amount of sample solution to a 50 mL volumetric flask. Dilute to the mark with ethyl acetate, shake and measure again. C.6 Preparation of standard solution
C.6.1 Standard solution: about 10 mg/mL
Weigh about 1 g (accurate to 0.1 m&) of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride respectively and place them in four 100 mL volumetric flasks, dilute to the mark with ethyl acetate, mix well, C.6.2 Standard solution; 500 μ/mL
Pipette an appropriate amount of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride standard solution respectively and place them in a 190 mL. Dilute to the mark with ethyl acetate in a volumetric flask and shake to obtain a standard solution of dimethane, 1,2-diethane, 1,1,2-diethylenetriamine and trifluoroethylene with a concentration of 500 μg/mL. C.6.3 Preparation of a series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place it in six 25 ml volumetric flasks, dilute to the mark with ethyl acetate and shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)Determination of adhesives for shoes and bags with a content of 2-dichloroethane, 1,1,2-trichloroethane and difluoroethane above 0.1 g/kg.
C.2 Principle
The sample is dissolved in an appropriate solvent, and the sample is injected into the sample chamber through a micro-injector, and then introduced into the chromatographic column. It is separated into corresponding components in the chromatographic column, and detected and recorded with a hydrogen flame ionization detector. The content of the measured components in the sample solution is calculated by the external standard method.
C.3 Reagents
C.3.1-Methylene chloride, 1,2-difluoroethane, 1,1,2-trichloroethane and dichloroethylene are all chromatographically pure. C.3.2 Acetate; analytically pure
C.4 Instrument
C.4.1 Injector: 5 μl micro-injector. C.4.2 Chromatography with hydrogen flame ionization detector. C.4.3 Chromatographic column: capillary column (50m×0.20nm×0.5um). The stationary liquid is polysiloxane. C.4.4 Recording device: integrator or chromatographic workstation. C.4.5 Determination conditions
Vaporization chamber temperature: 200°C+
C. 4. 5. 1
C, 4, 5, 2
Detection density: 250%
Nitrogen: purity greater than 99,999%, silica gel dehydration, column head pressure of 70 kPa30℃): C. 4. 5. 31
Hydrogen, purity greater than 99.999%, silica gel dehydration, column head pressure of 65 kPaC. 4. 5. 4
C. 4. 5. 5
Air: silica gel dehydration, column head pressure of 55 kPa: split, split ratio is 20:1:
C. 4. 5. 6:
Blowing: 30 ml.
C. 4. 5. 71
C. 4,5. 8 Program source
1st stage: initial temperature 30℃. Holding time 30min. Heating rate 2%℃/min, final temperature 60℃, 2nd stage: initial temperature 60%, holding time 0min. Heating rate 5℃/min, final temperature 90℃, 3rd stage: initial temperature 90%. Holding time 0min, heating rate 10~./min, final temperature 150℃. Holding time 11min.C.5 Analysis steps
Take (0.2 g~0.3% accurate to 0.1 Img) sample, microcentrifuge 0 ml. Dissolve in ethyl acetate and dilute to the mark. Shake well. [When the peaks of the measured components are difficult to separate due to other components, it is necessary to switch to this type of reagent and conduct the test under appropriate conditions. GB19340--2003
Use a 5L syringe to take 2.0μ1. Inject the sample and check its area. If the frontal area of the sample solution is larger than the peak area of the maximum concentration, use a pipette to transfer an appropriate amount of sample solution to a 50 mL volumetric flask. Dilute to the mark with ethyl acetate, shake and measure again. C.6 Preparation of standard solution
C.6.1 Standard solution: about 10 mg/mL
Weigh about 1 g (accurate to 0.1 m&) of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride respectively and place them in four 100 mL volumetric flasks, dilute to the mark with ethyl acetate, mix well, C.6.2 Standard solution; 500 μ/mL
Pipette an appropriate amount of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride standard solution respectively and place them in a 190 mL. Dilute to the mark with ethyl acetate in a volumetric flask and shake to obtain a standard solution of dimethane, 1,2-diethane, 1,1,2-diethylenetriamine and trifluoroethylene with a concentration of 500 μg/mL. C.6.3 Preparation of a series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place it in six 25 ml volumetric flasks, dilute to the mark with ethyl acetate and shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)Determination of adhesives for shoes and bags with a content of 2-dichloroethane, 1,1,2-trichloroethane and difluoroethane above 0.1 g/kg.
C.2 Principle
The sample is dissolved in an appropriate solvent, and the sample is injected into the sample chamber through a micro-injector, and then introduced into the chromatographic column. It is separated into corresponding components in the chromatographic column, and detected and recorded with a hydrogen flame ionization detector. The content of the measured components in the sample solution is calculated by the external standard method.
C.3 Reagents
C.3.1-Methylene chloride, 1,2-difluoroethane, 1,1,2-trichloroethane and dichloroethylene are all chromatographically pure. C.3.2 Acetate; analytically pure
C.4 Instrument
C.4.1 Injector: 5 μl micro-injector. C.4.2 Chromatography with hydrogen flame ionization detector. C.4.3 Chromatographic column: capillary column (50m×0.20nm×0.5um). The stationary liquid is polysiloxane. C.4.4 Recording device: integrator or chromatographic workstation. C.4.5 Determination conditions
Vaporization chamber temperature: 200°C+
C. 4. 5. 1
C, 4, 5, 2
Detection density: 250%
Nitrogen: purity greater than 99,999%, silica gel dehydration, column head pressure of 70 kPa30℃): C. 4. 5. 31
Hydrogen, purity greater than 99.999%, silica gel dehydration, column head pressure of 65 kPaC. 4. 5. 4
C. 4. 5. 5
Air: silica gel dehydration, column head pressure of 55 kPa: split, split ratio is 20:1:
C. 4. 5. 6:
Blowing: 30 ml.
C. 4. 5. 71
C. 4,5. 8 Program source
1st stage: initial temperature 30℃. Holding time 30min. Heating rate 2%℃/min, final temperature 60℃, 2nd stage: initial temperature 60%, holding time 0min. Heating rate 5℃/min, final temperature 90℃, 3rd stage: initial temperature 90%. Holding time 0min, heating rate 10~./min, final temperature 150℃. Holding time 11min.C.5 Analysis steps
Take (0.2 g~0.3% accurate to 0.1 Img) sample, microcentrifuge 0 ml. Dissolve in ethyl acetate and dilute to the mark. Shake well. [When the peaks of the measured components are difficult to separate due to other components, it is necessary to switch to this type of reagent and conduct the test under appropriate conditions. GB19340--2003
Use a 5L syringe to take 2.0μ1. Inject the sample and check its area. If the frontal area of the sample solution is larger than the peak area of the maximum concentration, use a pipette to transfer an appropriate amount of sample solution to a 50 mL volumetric flask. Dilute to the mark with ethyl acetate, shake and measure again. C.6 Preparation of standard solution
C.6.1 Standard solution: about 10 mg/mL
Weigh about 1 g (accurate to 0.1 m&) of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride respectively and place them in four 100 mL volumetric flasks, dilute to the mark with ethyl acetate, mix well, C.6.2 Standard solution; 500 μ/mL
Pipette an appropriate amount of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and vinyl chloride standard solution respectively and place them in a 190 mL. Dilute to the mark with ethyl acetate in a volumetric flask and shake to obtain a standard solution of dimethane, 1,2-diethane, 1,1,2-diethylenetriamine and trifluoroethylene with a concentration of 500 μg/mL. C.6.3 Preparation of a series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place it in six 25 ml volumetric flasks, dilute to the mark with ethyl acetate and shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)2-Dichloroethane and 1,2-dichloroethane and 1,1,2-trichloroethane are placed in four 100mL volumetric flasks, diluted to the mark with ethyl acetate, shake well, C.6.2 Standard solution; 500 μ/mL
Take appropriate volume of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and 1,6,1-trichloroethane respectively, place in a 190mL volumetric flask, dilute to the mark with ethyl acetate, shake to obtain the standard solution of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and 1,6,1-trifluoroethylene with the concentration of 500μg/mL. C.6.3 Preparation of series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place in six 25mL volumetric flasks, dilute to the mark with ethyl acetate, shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)2-Dichloroethane and 1,2-dichloroethane and 1,1,2-trichloroethane are placed in four 100mL volumetric flasks, diluted to the mark with ethyl acetate, shake well, C.6.2 Standard solution; 500 μ/mL
Take appropriate volume of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and 1,6,1-trichloroethane respectively, place in a 190mL volumetric flask, dilute to the mark with ethyl acetate, shake to obtain the standard solution of dichloromethane, 1,2-dichloroethane, 1,1,2-trichloroethane and 1,6,1-trifluoroethylene with the concentration of 500μg/mL. C.6.3 Preparation of series of standard solutions
Take the volume of standard solution (t6.2) listed in C.1 and place in six 25mL volumetric flasks, dilute to the mark with ethyl acetate, shake well:
Table (. 1. Volume of a series of standard solutions and corresponding concentrations. Volume transferred
Change of ammonia
(re:iml.)
(.6.4 Determination of peak area of a series of standard solutions 1.?…Concentration of ethyl chloride
[.Concentration of 1,2-ethyl chloride
Concentration of vinyl chloride
Non-phase chromatograph, set the chromatographic conditions, wait for the line to stabilize, use a μI. syringe to take 2.0 μI Inject standard solutions and measure the peak area. Each standard solution is sampled twice and the average value is taken. C.6.5 Drawing of the standard curve
Use the peak area A of dichloromethane, 1.2-dichloroethane, 1,1,2-trichloroethane and trichloroethylene as the vertical axis and the concentration c (μgmL) of the corresponding standard solution as the horizontal axis. Draw the standard curves of dichloromethane, 1.2-dichloroethane, 1,1,2-dichloroethane and 3-chloroethylene. C.7 Expression of results
Read directly from the standard curve or calculate according to the normalization equation The concentration of the component to be tested in the sample solution. The content of the component to be tested in the sample, X, is calculated as follows: cvf
X-10gm
Wu:
X——-the content of the component to be tested in the sample, in grams per dry gram (gkg); the concentration of the component to be tested in the sample solution, in grams per liter (μg/ml.): V--the volume of the sample solution, in milliliters (ml.) n----the mass of the sample, in grams (g):-the dilution multiple of the sample solution.
.(. 1)
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