This standard specifies the limits of harmful substances in adhesives for indoor building decoration and renovation and their test methods. This standard applies to adhesives for indoor building decoration and renovation. GB 18583-2001 Limits of harmful substances in adhesives for indoor decoration and renovation materials GB18583-2001 Standard download decompression password: www.bzxz.net

ICS83.180
National Standard of the People's Republic of China
GB 18583—2001
Indoor decorating and refurbishing materials---Limit ofharmful substances of adhesives2001-12-10 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Implementation on 2002-01-01
GB18583—2001
Chapter 3 of this standard is mandatory, and the rest are recommended clauses. Introduction
Appendices A, B, C, D and E of this standard are normative appendices. From January 1, 2002, the products produced by the production enterprises shall comply with this national standard, with a transition period of 6 months; from July 1, 2002, the products that do not meet this national standard shall be stopped from being sold in the market. This standard is proposed by the China Petroleum and Chemical Industry Association. This standard is under the jurisdiction of the National Technical Committee for Standardization of Adhesives. The responsible drafting units of this standard are: Shanghai Rubber Products Research Institute, Sinochem Chemical Standardization Institute, Environmental Sanitation Testing Institute of Chinese Academy of Preventive Medicine, and China Adhesives Industry Association. The participating drafting units of this standard are: Fushun Hele Chemical Co., Ltd., Henkel Adhesive Co., Ltd., Shenzhen Guqiang Adhesive Co., Ltd., Shanghai Donghe Adhesive Co., Ltd., and Jiangsu Hesonglin Adhesive Factory. The drafters of this standard are: Wang Dinglin, Jin Weixing, Mei Jian, Xu Dongqun, Shen Yihua, Li Xianquan, Shi Yuxiang, and Gong Beifan. This standard is entrusted to the National Technical Committee for Standardization of Adhesives for interpretation. This standard was first issued on December 10, 2001. 486
1 Scope
Indoor decoration and renovation materials
Limits of harmful substances in adhesives
This standard specifies the limits of harmful substances in adhesives for indoor architectural decoration and renovation and their test methods. This standard applies to adhesives for indoor architectural decoration and renovation. 2 Normative references
GB 18583--2001
The clauses in the following documents become the clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, the parties to an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version shall apply to this standard. GB/T601--1988 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T606—1988 General method for determination of water content in chemical reagents (Karl Fischer method) (eqvISO6353-1:1982) GB/T 2793—1995
Determination of non-volatile matter content of adhesives
GB/T 13354—1992
3 Requirements
Determination of density of liquid adhesives Gravimetric cup method 3.1 The limit values ​​of harmful substances in solvent-based adhesives shall comply with the provisions of Table 1. Table 1 Limit values ​​of harmful substances in solvent-based adhesives Item
Free formaldehyde/(g/kg)
Benzene\/(g/kg)
Toluene + xylene/(g/kg)
Toluene diisocyanate/(g/kg)
Total volatile organic matter/(g/L)
Rubber adhesive
Polyurethane adhesive
Note: 1) Benzene cannot be used as a solvent, and its maximum content as an impurity shall not exceed the provisions of Table 1. 3.2
The limit values ​​of harmful substances in water-based adhesives shall comply with the provisions of Table 2. Table 2 Limit values ​​of harmful substances in water-based adhesives refer to
Free formaldehyde/(g/kg)
Benzene/(g/kg)
Toluene and dodecene/(g/kg)
Total volatile organic matter/(g/L)
Formal
Adhesive
Polyvinyl acetate
Adhesive
Rubber
Adhesive
Other adhesives
Polyurethane
Adhesive
Other adhesives
GB18583--2001
4 Test methods
4.1 The determination of free formaldehyde content shall be carried out in accordance with Appendix A; 4.2 The determination of benzene content shall be carried out in accordance with Appendix B; 4.3 The determination of toluene and xylene content shall be carried out in accordance with Appendix C; 4.4 The determination of free toluene diisocyanate content shall be carried out in accordance with Appendix D; 4.5 The determination of total volatile organic compound content shall be carried out in accordance with Appendix E. 5 Inspection rules
5.1 Type inspection
All requirements listed in this standard are type inspection items. Under normal circumstances, type inspection shall be carried out at least once a year. Type inspection shall be carried out when there are major changes in production formula, process and raw materials or when production is resumed after suspension for three months. 5.2 Sampling method
Three samples shall be randomly selected from the same batch of products, each of which shall not be less than 0.5kg. 5.3 Determination of test results
One of the three samples is taken and tested according to the provisions of this standard. If the test results of all items meet the requirements of this standard, it is judged to be qualified. If one of the test results does not meet the requirements of this standard, the preserved sample should be retested. If the result still does not meet the requirements of this standard, it is judged to be unqualified. 6 Packaging mark
Adhesive products used for interior decoration materials must indicate the name and content of harmful substances specified in this standard on the packaging. 7 Test report
The test report should include the following contents:
a) The name and number of this standard;
b) The name, production unit and batch number of the sample;
d) The name and model of the instrument used;
e) Test results;
f) Abnormal conditions that occur during the test; g) The inspector and the test date.
A.1 Scope
Appendix A
(Normative Appendix)
Determination of free formaldehyde content in adhesives Acetylacetone spectrophotometric method This method is applicable to the determination of free formaldehyde content in adhesives for indoor building decoration and renovation. This method is applicable to adhesives for indoor building decoration and renovation with a free formaldehyde content greater than 0.005%. A.2 Principle
GB18583.-2001
Water-based adhesives are dissolved in water, and surface solvent adhesives are first dissolved in ethyl acetate and then dissolved in water. Under acidic conditions, the free formaldehyde dissolved in water is evaporated with water. In the acetic acid-ammonium acetate buffer solution of pH=6, the formaldehyde in the distillate reacts with acetylacetone to quickly generate a stable yellow compound under boiling water bath conditions, and its absorbance is measured at 415.40nm after cooling. According to the standard curve, the free formaldehyde content in the sample is calculated.
A.3 Reagents
Unless otherwise specified, only reagents confirmed as analytically pure and distilled water or deionized water or water of equivalent purity shall be used in the analysis. A.3.1 Ammonium acetate;
A.3.2 Glacial acetic acid: p=1.055g/mL;
A.3.3 Acetylacetone: p=0.975g/mL; A.3.3.1 Acetylacetone solution: 0.25% (volume fraction), weigh 25g ammonium acetate (A.3.1), add a small amount of water to dissolve, add 3ml glacial acetic acid (A.3.2) and 0.25mL acetylacetone (A.3.3), mix and then add water to 100mL, adjust pH=6.0, this solution is stored at pH2~~5 and can be stable for one month.
A.3.4 Hydrochloric acid solution: 1+5(V+V);Www.bzxZ.net
A.3.5 Sodium hydroxide solution: 30g/100mL;A.3.6 Iodine (I2);
A.3.6.1 Iodine solution: c(I2)=0.1mol/L, prepared according to GB/T601-1988;A.3.7 Sodium thiosulfate solution: c(Na2S,O.)=0.1mol/L, prepared according to GB/T601-1988. A.3.8 Starch solution: 1g/100mL, weigh 1g starch, mix it into a paste with a small amount of water, pour it into 100ml boiling water, it will be a transparent solution, prepared before use.
A.3.9 Formaldehyde: mass fraction is 36%~38%; A.3.9.1 Formaldehyde standard stock solution: take 10mL formaldehyde solution (A.3.9) and place it in a 500mL volumetric flask, and dilute it to the mark with water. A.3.9.2 Calibration of formaldehyde standard stock solution: take 5.0ml. formaldehyde standard stock solution (A.3.9.1) and place it in a 250ml iodine volumetric flask, add 0.1mol/L iodine solution (A.3.6.1)30.0mL, immediately add 30g/100mL sodium hydroxide solution (A.3.5) dropwise until the color fades to light yellow (about 0.7mL). Let stand for 10min, add 15ml hydrochloric acid solution (A.3.4), let stand in the dark for 10min, add 100mL freshly boiled but cooled water, titrate with calibrated sodium thiosulfate solution (A, 3.7) until light yellow, add 1mL of newly prepared 1g/100mL starch indicator (A.3.8), and continue titrating until the blue color just disappears as the end point. Perform blank determination at the same time. Calculate the concentration of formaldehyde standard stock solution Cformaldehyde according to formula (A.1). C year acid
(VV,)cX15. 0
GB 18583-2001
Wherein:
C formaldehyde
concentration of formaldehyde standard stock solution, in milligrams per milliliter (mg/mL); V,---volume of sodium thiosulfate solution consumed by blank, in milliliters (mL); V2-volume of sodium thiosulfate solution consumed by standard formaldehyde, in milliliters (mL); concentration of sodium thiosulfate solution, in moles per liter (mol/L); c
molar mass of formaldehyde (1/2HCHO);
5. 0--sample volume of formaldehyde standard stock solution, in milliliters (mL). A.3.9.3 Formaldehyde standard solution: dilute the formaldehyde standard stock solution (A.3.9.1) with water to a 10.0ug/mL formaldehyde standard solution. Store at 2C-5C and it is stable for one week.
A.3.10 Phosphoric acid;
A.3.11 Ethyl acetate.
A.4 Apparatus
Single-mouth distillation flask: 500mL;
Straight condenser;
A.4.3 Volumetric flask: 250mL, 200mL, 25mL;A.4.4 Water bath;
Spectrophotometer.
A.5 Analysis steps
A.5.1 Drawing of standard curve
According to the volume of formaldehyde standard stock solution listed in Table A.1, add 5mL of 0.25% acetylacetone solution (A.3.3.1) to six 25mL volumetric flasks (A.4.3), dilute to the mark with water, mix well, heat in boiling water for 3min, take out and cool to room temperature, use a 1cm absorption cell, take blank solution as reference, measure absorbance at wavelength 415nm, take absorbance A as ordinate and formaldehyde concentration c (μg/mL) as abscissa, draw a standard curve, or calculate its regression equation by least square method. Table A. 1 Volume of standard solution and corresponding formaldehyde concentration Formaldehyde standard solution (A.3.9.3)
Note: 1) Blank solution.
A.5.2 Sample determination
A.5.2.1 Water-based adhesive
Corresponding formaldehyde concentration
(μg/mL)
Weigh 5.0g of sample (accurate to 0.1mg), place it in a 500mL distillation flask, add 250mL of water to dissolve it, then add 5mL of phosphoric acid and shake well.
Install the distillation apparatus, distill in an oil bath, and stop distilling until the distillate is 200mL. Transfer the distillate to a 250mL volumetric flask and dilute it to the mark with water. Take 10ml of the distillate and put it in a 25mL volumetric flask, add 5mL of acetylacetone solution (A.3.3.1), dilute it to the mark with water, and shake well. Boil it in a boiling water bath for 3min, take it out and cool it to room temperature. Then measure its absorbance. A.5.2.2 Solvent-based adhesives
GB18583--2001
Weigh 5.0g of the sample (accurate to 0.1mg), place it in a 500mL distillation flask, add 20mL of ethyl acetate (A.3.11) to dissolve, then add 250mL of water, then add 5mL of phosphoric acid, and shake. Install the distillation apparatus, distill in an oil bath, and stop distilling until the distillate is 200mL. Transfer the distillate to a 250mL volumetric flask and dilute it to the mark with water. Take 10mL of the distillate in a 25mL volumetric flask, add 5ml of acetylacetone solution (A.3.3.1), dilute it to the mark with water, and shake it well. Place it in a boiling water bath and boil for 3min, take it out and cool it to room temperature. Then measure its absorbance. A.6 Result expression
Read the formaldehyde concentration of the sample solution directly from the standard curve. The free formaldehyde content X in the sample is calculated by the formula: X
Wherein:
(c.—ch)Vf
X—free formaldehyde content, in grams per kilogram (g/kg); c-formaldehyde concentration in the sample solution read from the standard curve, in micrograms per milliliter (ug/mL); Cb-
~formaldehyde concentration in the blank solution read from the standard curve, in micrograms per milliliter (μg/mL); V—volume of the distillate after constant volume, in milliliters (mL); m-—mass of the sample, in grams (g); f-—dilution factor of the sample solution.
GB 18583--2001
B.1 Scope
Appendix B
(Normative Appendix)
Determination of benzene content in adhesives Gas chromatography This method specifies the method for determining the benzene content in adhesives for indoor building decoration and renovation. This method is applicable to adhesives for indoor building decoration and renovation with a benzene content of more than 0.02g/kg. B.2 Principle
After the sample is diluted with an appropriate solvent, the diluted sample solution is directly injected into the injection device using a micro syringe and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column and detected and recorded with a hydrogen flame ionization detector. The benzene content in the sample solution is calculated using the external standard method.
B.3 Reagents
B.3.1 Benzene: chromatographic grade;
B.3.2 N,N-dimethylformamide: analytical grade. B.4 Instruments
Injector: 5μL micro-syringe;
Chromatograph: with hydrogen flame ionization detector; Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; B.4.3
Recording device: integrator or chromatographic workstation; B.4.5 Determination conditions
B.4.5.1 Vaporization chamber temperature: 200C;
B.4.5.2 Detection chamber temperature: 25 0C;
B.4.5.3 Nitrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 70kPa (30℃);B.4.5.4 Hydrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 65kPa; Air: dehydrated with silica gel, column head pressure of 55kPa;B.4.5.5
B.4.5.6 Program temperature rise: initial temperature 30℃, holding time 3min, heating rate 20℃/min, final temperature 150C, holding time 5min.
B.5 Analysis steps
Weigh 0.2g~0.3g (accurate to 0.1mg) of the sample, place it in a 50ml volumetric flask, dissolve it with N,N-dimethylformamide and dilute to the scale, shake well. Take 2μL of the sample with a 5μuL syringe and measure its peak area. If the peak area of ​​the sample solution is greater than the peak area of ​​the maximum concentration in Table 1, use a pipette to accurately transfer V volume of the sample solution to a 50mL volumetric flask, dilute to the mark with N,N-dimethylformamide, shake well and then measure again.
B.6 Preparation of standard solutions
B.6.1 Benzene standard solution: 1.0 mg/mL
Weigh 0.1000g of benzene, place it in a 100mL volumetric flask, dilute to the mark with N,N-dimethylformamide, and shake well. 492
B. 6.2 Dosage of series of benzene standard solutions
GB18583--2001
According to the volume of the benzene standard solution (B.6.1) listed in Table B.1, add it to six 25mL volumetric flasks respectively, dilute to the mark with N,N-dimethylformamide, and shake well.
Table B.1 Volume of a series of standard solutions and corresponding benzene concentrations Volume transferred
B.6.3 Determination of peak area of ​​a series of standard solutions Corresponding benzene concentration
(μg/mL)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to inject 2uL of the standard solution and measure the peak area. Inject each standard solution five times and take the average value. B.6.4 Drawing of the standard curve
Use the peak area A as the ordinate and the corresponding concentration c (μg/mL) as the abscissa to obtain the standard curve. B.7 Expression of results
Read the concentration of benzene in the sample solution directly from the standard curve. The benzene content in the sample is X,The calculation formula is:
Wherein:
X—toluene content in the sample, in grams per kilogram (g/kg);-benzene concentration in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); Gi
volume of the sample solution, in milliliters (ml); m—mass of the sample, in grams (g); dilution factor.
GB 18583--2001
C.1 Scope
Appendix C
(Normative Appendix)
Determination of toluene and xylene content in adhesives Gas chromatography
This method specifies the method for determining the toluene and xylene content in adhesives for indoor building decoration and renovation. This method is applicable to adhesives for indoor building decoration and renovation with a toluene content of more than 0.02g/kg. This method is applicable to adhesives for indoor building decoration and renovation with a xylene content of more than 0.02g/kg. C.2 Principle
After the sample is diluted with an appropriate solvent, the diluted sample solution is directly injected into the injection device with a micro-syringe and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column and detected and recorded with a hydrogen flame ionization detector. The content of toluene and xylene in the sample solution is calculated by the external standard method. C.3 Reagents
C.3.1 Toluene: chromatographically pure;
C.3.2 Meta-xylene and para-xylene: chromatographically pure; C.3.3 Ortho-xylene: chromatographically pure;
C.3.4 Ethyl acetate: analytically pure.
C.4 Instruments
C.4.1 Injection device: 5μl micro-syringe; C.4.2#
Chromatograph: with hydrogen flame ionization detector; C.4.3 Chromatographic column: large-bore capillary column: DB-1 (30mX0.53mm×1.5μm), the stationary liquid is dimethylpolysiloxane; C.4.4 Recording device: integrator or chromatographic workstation; C.4.5 Determination conditions
C.4.5.1 Vaporization chamber temperature: 200℃;
C.4. 5.2 Test chamber temperature: 250C;
C.4.5.3 Nitrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 70kPa (30C);C.4.5.4 Hydrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 65kPa;C.4.5.5 Air: dehydrated with silica gel, column head pressure of 55kPa;C.4.5.6 Program temperature rise: initial temperature 35C, holding time 2min, heating rate 20C/min, final temperature 150C, holding time 5min.
C.5 Analysis steps
Weigh 0.2g~0.3g (accurate to 0.1mg) of the sample, place it in a 50mL volumetric flask, dissolve it with ethyl acetate and dilute to the mark, shake well. Take 2μL of the sample with a 5L syringe and measure its peak area. If the peak area of ​​the sample solution is greater than the peak area of ​​the maximum concentration in the table, use a pipette to accurately transfer V volume of the sample solution to a 50mL volumetric flask, dilute to the mark with ethyl acetate, shake and then measure. 494
C.6 Preparation of standard solutions
GB18583--2001
C. 6.1 Toluene, m-xylene, p-xylene, o-xylene standard solutions: 1. 0 mg/mL, 1. 0 mg/mL, 1. 0 mg/mL Weigh 0.1000g toluene, 0.1000g m-xylene, p-xylene, and 0.1000g o-xylene, place in a 100ml volumetric flask, dilute to the mark with ethyl acetate, and shake well. C.6.2 Preparation of series of standard solutions
Add the volumes of standard solutions (B.6.1) listed in Table C.1 to six 25mL volumetric flasks, dilute to scale with ethyl acetate, and shake well.
Table C.1 Volumes and corresponding concentrations of standard solutions (B.6.1)Transferred volume
Corresponding concentration of toluene
(μg/mL)
C.6.3 Determination of peak areas of series of standard solutionsCorresponding concentrations of m-xylene and
p-xylene
(μg/mL)
Corresponding concentration of o-xylene
(μg/mL)
Start the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to take 2uL of standard solution for injection and measure the peak area. Inject each standard solution five times and take the average value. C.6.4 Drawing of standard curve
Use peak area A as ordinate and corresponding concentration c (μg/mL) as abscissa to obtain standard curve. C.7 Expression of results
Read the concentration of toluene or xylene in the sample solution directly from the standard curve. The content of toluene or xylene in the sample X, the sieve counting formula is: X:
Where:
X--the content of toluene or xylene in the sample, in grams per kilogram (g/kg); Ct
The concentration of toluene or xylene in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); the volume of the sample solution, in milliliters (mL); the mass of the sample, in grams (g);
-dilution factor.
GB18583—2001
D.1 Scope
Appendix D
(Normative Appendix)
Determination of free toluene diisocyanate content in polyurethane adhesives Gas chromatography
This method is applicable to the determination of free toluene diisocyanate content in polyurethane adhesives for indoor building decoration and renovation. This method can determine polyurethane adhesives for indoor building decoration and renovation with a free toluene diisocyanate content of more than 0.1g/kg. D.2 Principle
After the sample is diluted with an appropriate solvent, n-tetradecane is added as an internal standard. The diluted sample solution is injected into the injection device and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column, detected and recorded with a hydrogen flame ionization detector, and the content of toluene diisocyanate in the sample solution is calculated by the internal standard method. D.3 Reagents
D.3.1 Ethyl acetate: add 100g 5A molecular sieve (D.3.4), filter after leaving for 24h; D.3.2 Toluene diisocyanate;
D.3.3 n-Tetradecane: chromatographic grade;
D.3.4 5A molecular sieve: heat in a high temperature furnace at 500C for 2h, cool in a desiccator for later use. D.4 Instruments
D.4.1 Injection device: 5μL micro-syringe; D.4.2 Chromatograph: with hydrogen flame ionization detector; D.4.3 Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; D.4.4 Recording device: integrator or chromatographic workstation; D.4.5 Determination conditions
D.4.5.1 Vaporization chamber temperature: 16 0C;
D.4.5.2 Detection room temperature: 200C;
D.4.5.3 Column box temperature: 135℃;
D.4.5.4 Nitrogen: purity greater than 99.9%, column head pressure 100kPa (135℃); D.4.5.5 Hydrogen: purity greater than 99.9%. Silica gel dehydration, column head pressure 65kPa; D.4.5.6 Air: Silica gel dehydration, column head pressure 55kPa. D.5 Analysis steps
D.5.1 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g toluene diisocyanate in a 50mL volumetric flask, add 5ml internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4962 Principle
After the sample is diluted with an appropriate solvent, the diluted sample solution is directly injected into the injection device with a micro-syringe, and is carried into the chromatographic column by the carrier gas, where it is separated into corresponding components. The chromatogram is detected and recorded with a hydrogen flame ionization detector, and the content of toluene and xylene in the sample solution is calculated using the external standard method. C.3 Reagents
C.3.1 Toluene: chromatographically pure;
C.3.2 m-xylene and p-xylene: chromatographically pure; C.3.3 o-xylene: chromatographically pure;
C.3.4 Ethyl acetate: analytically pure.
C.4 Instruments
C.4.1 Injection device: 5μl micro-syringe; C.4.2#
Chromatograph: with hydrogen flame ionization detector; C.4.3 Chromatographic column: large-bore capillary column: DB-1 (30mX0.53mm×1.5μm), the stationary liquid is dimethylpolysiloxane; C.4.4 Recording device: integrator or chromatographic workstation; C.4.5 Determination conditions
C.4.5.1 Vaporization chamber temperature: 200℃;
C.4. 5.2 Test chamber temperature: 250C;
C.4.5.3 Nitrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 70kPa (30C);C.4.5.4 Hydrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 65kPa;C.4.5.5 Air: dehydrated with silica gel, column head pressure of 55kPa;C.4.5.6 Program temperature rise: initial temperature 35C, holding time 2min, heating rate 20C/min, final temperature 150C, holding time 5min.
C.5 Analysis steps
Weigh 0.2g~0.3g (accurate to 0.1mg) of the sample, place it in a 50mL volumetric flask, dissolve it with ethyl acetate and dilute to the mark, shake well. Take 2μL of the sample with a 5L syringe and measure its peak area. If the peak area of ​​the sample solution is greater than the peak area of ​​the maximum concentration in the table, use a pipette to accurately transfer V volume of the sample solution to a 50mL volumetric flask, dilute to the mark with ethyl acetate, shake and then measure. 494
C.6 Preparation of standard solutions
GB18583--2001
C. 6.1 Toluene, m-xylene, p-xylene, o-xylene standard solutions: 1. 0 mg/mL, 1. 0 mg/mL, 1. 0 mg/mL Weigh 0.1000g toluene, 0.1000g m-xylene, p-xylene, and 0.1000g o-xylene, place in a 100ml volumetric flask, dilute to the mark with ethyl acetate, and shake well. C.6.2 Preparation of series of standard solutions
Add the volumes of standard solutions (B.6.1) listed in Table C.1 to six 25mL volumetric flasks, dilute to scale with ethyl acetate, and shake well.
Table C.1 Volumes and corresponding concentrations of standard solutions (B.6.1)Transferred volume
Corresponding concentration of toluene
(μg/mL)
C.6.3 Determination of peak areas of series of standard solutionsCorresponding concentrations of m-xylene and
p-xylene
(μg/mL)
Corresponding concentration of o-xylene
(μg/mL)
Start the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to take 2uL of standard solution for injection and measure the peak area. Inject each standard solution five times and take the average value. C.6.4 Drawing of standard curve
Use peak area A as ordinate and corresponding concentration c (μg/mL) as abscissa to obtain standard curve. C.7 Expression of results
Read the concentration of toluene or xylene in the sample solution directly from the standard curve. The content of toluene or xylene in the sample X, the sieve counting formula is: X:
Where:
X--the content of toluene or xylene in the sample, in grams per kilogram (g/kg); Ct
The concentration of toluene or xylene in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); the volume of the sample solution, in milliliters (mL); the mass of the sample, in grams (g);
-dilution factor.
GB18583—2001
D.1 Scope
Appendix D
(Normative Appendix)
Determination of free toluene diisocyanate content in polyurethane adhesives Gas chromatography
This method is applicable to the determination of free toluene diisocyanate content in polyurethane adhesives for indoor building decoration and renovation. This method can determine polyurethane adhesives for indoor building decoration and renovation with a free toluene diisocyanate content of more than 0.1g/kg. D.2 Principle
After the sample is diluted with an appropriate solvent, n-tetradecane is added as an internal standard. The diluted sample solution is injected into the injection device and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column, detected and recorded with a hydrogen flame ionization detector, and the content of toluene diisocyanate in the sample solution is calculated by the internal standard method. D.3 Reagents
D.3.1 Ethyl acetate: add 100g 5A molecular sieve (D.3.4), filter after leaving for 24h; D.3.2 Toluene diisocyanate;
D.3.3 n-Tetradecane: chromatographic grade;
D.3.4 5A molecular sieve: heat in a high temperature furnace at 500C for 2h, cool in a desiccator for later use. D.4 Instruments
D.4.1 Injection device: 5μL micro-syringe; D.4.2 Chromatograph: with hydrogen flame ionization detector; D.4.3 Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; D.4.4 Recording device: integrator or chromatographic workstation; D.4.5 Determination conditions
D.4.5.1 Vaporization chamber temperature: 16 0C;
D.4.5.2 Detection room temperature: 200C;
D.4.5.3 Column box temperature: 135℃;
D.4.5.4 Nitrogen: purity greater than 99.9%, column head pressure 100kPa (135℃); D.4.5.5 Hydrogen: purity greater than 99.9%. Silica gel dehydration, column head pressure 65kPa; D.4.5.6 Air: Silica gel dehydration, column head pressure 55kPa. D.5 Analysis steps
D.5.1 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g toluene diisocyanate in a 50mL volumetric flask, add 5ml internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4962 Principle
After the sample is diluted with an appropriate solvent, the diluted sample solution is directly injected into the injection device with a micro-syringe, and is carried into the chromatographic column by the carrier gas, where it is separated into corresponding components. The chromatogram is detected and recorded with a hydrogen flame ionization detector, and the content of toluene and xylene in the sample solution is calculated using the external standard method. C.3 Reagents
C.3.1 Toluene: chromatographically pure;
C.3.2 m-xylene and p-xylene: chromatographically pure; C.3.3 o-xylene: chromatographically pure;
C.3.4 Ethyl acetate: analytically pure.
C.4 Instruments
C.4.1 Injection device: 5μl micro-syringe; C.4.2#
Chromatograph: with hydrogen flame ionization detector; C.4.3 Chromatographic column: large-bore capillary column: DB-1 (30mX0.53mm×1.5μm), the stationary liquid is dimethylpolysiloxane; C.4.4 Recording device: integrator or chromatographic workstation; C.4.5 Determination conditions
C.4.5.1 Vaporization chamber temperature: 200℃;
C.4. 5.2 Test chamber temperature: 250C;
C.4.5.3 Nitrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 70kPa (30C);C.4.5.4 Hydrogen: purity greater than 99.9%, dehydrated with silica gel, column head pressure of 65kPa;C.4.5.5 Air: dehydrated with silica gel, column head pressure of 55kPa;C.4.5.6 Program temperature rise: initial temperature 35C, holding time 2min, heating rate 20C/min, final temperature 150C, holding time 5min.
C.5 Analysis steps
Weigh 0.2g~0.3g (accurate to 0.1mg) of the sample, place it in a 50mL volumetric flask, dissolve it with ethyl acetate and dilute to the mark, shake well. Take 2μL of the sample with a 5L syringe and measure its peak area. If the peak area of ​​the sample solution is greater than the peak area of ​​the maximum concentration in the table, use a pipette to accurately transfer V volume of the sample solution to a 50mL volumetric flask, dilute to the mark with ethyl acetate, shake and then measure. 494
C.6 Preparation of standard solutions
GB18583--2001
C. 6.1 Toluene, m-xylene, p-xylene, o-xylene standard solutions: 1. 0 mg/mL, 1. 0 mg/mL, 1. 0 mg/mL Weigh 0.1000g toluene, 0.1000g m-xylene, p-xylene, and 0.1000g o-xylene, place in a 100ml volumetric flask, dilute to the mark with ethyl acetate, and shake well. C.6.2 Preparation of series of standard solutions
Add the volumes of standard solutions (B.6.1) listed in Table C.1 to six 25mL volumetric flasks, dilute to scale with ethyl acetate, and shake well.
Table C.1 Volumes and corresponding concentrations of standard solutions (B.6.1)Transferred volume
Corresponding concentration of toluene
(μg/mL)
C.6.3 Determination of peak areas of series of standard solutionsCorresponding concentrations of m-xylene and
p-xylene
(μg/mL)
Corresponding concentration of o-xylene
(μg/mL)
Start the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to take 2uL of standard solution for injection and measure the peak area. Inject each standard solution five times and take the average value. C.6.4 Drawing of standard curve
Use peak area A as ordinate and corresponding concentration c (μg/mL) as abscissa to obtain standard curve. C.7 Expression of results
Read the concentration of toluene or xylene in the sample solution directly from the standard curve. The content of toluene or xylene in the sample X, the sieve counting formula is: X:
Where:
X--the content of toluene or xylene in the sample, in grams per kilogram (g/kg); Ct
The concentration of toluene or xylene in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); the volume of the sample solution, in milliliters (mL); the mass of the sample, in grams (g);
-dilution factor.
GB18583—2001
D.1 Scope
Appendix D
(Normative Appendix)
Determination of free toluene diisocyanate content in polyurethane adhesives Gas chromatography
This method is applicable to the determination of free toluene diisocyanate content in polyurethane adhesives for indoor building decoration and renovation. This method can determine polyurethane adhesives for indoor building decoration and renovation with a free toluene diisocyanate content of more than 0.1g/kg. D.2 Principle
After the sample is diluted with an appropriate solvent, n-tetradecane is added as an internal standard. The diluted sample solution is injected into the injection device and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column, detected and recorded with a hydrogen flame ionization detector, and the content of toluene diisocyanate in the sample solution is calculated by the internal standard method. D.3 Reagents
D.3.1 Ethyl acetate: add 100g 5A molecular sieve (D.3.4), filter after leaving for 24h; D.3.2 Toluene diisocyanate;
D.3.3 n-Tetradecane: chromatographic grade;
D.3.4 5A molecular sieve: heat in a high temperature furnace at 500C for 2h, cool in a desiccator for later use. D.4 Instruments
D.4.1 Injection device: 5μL micro-syringe; D.4.2 Chromatograph: with hydrogen flame ionization detector; D.4.3 Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; D.4.4 Recording device: integrator or chromatographic workstation; D.4.5 Determination conditions
D.4.5.1 Vaporization chamber temperature: 16 0C;
D.4.5.2 Detection room temperature: 200C;
D.4.5.3 Column box temperature: 135℃;
D.4.5.4 Nitrogen: purity greater than 99.9%, column head pressure 100kPa (135℃); D.4.5.5 Hydrogen: purity greater than 99.9%. Silica gel dehydration, column head pressure 65kPa; D.4.5.6 Air: Silica gel dehydration, column head pressure 55kPa. D.5 Analysis steps
D.5.1 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g toluene diisocyanate in a 50mL volumetric flask, add 5ml internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4966.1 Toluene, m-xylene, p-xylene, o-xylene standard solutions: 1.0 mg/mL, 1.0 mg/mL, 1.0 mg/mL Weigh 0.1000g toluene, 0.1000g m-xylene, p-xylene, 0.1000g o-xylene, place in a 100ml volumetric flask, dilute to scale with ethyl acetate, and shake well. C.6.2 Preparation of series standard solutions
According to the volume of standard solution (B.6.1) listed in Table C.1, add them to six 25mL volumetric flasks respectively, dilute to scale with ethyl acetate, and shake well.
Table C.1 Volume of standard solution (B.6.1) and corresponding concentration Volume transferred
Corresponding toluene concentration
(μg/mL)
C.6.3 Determination of peak area of ​​series of standard solutions Corresponding tom-xylene and
p-xylene concentration
(μg/mL)
Corresponding too-xylene concentration
(μg/mL)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to inject 2uL of standard solution and measure the peak area. Inject each standard solution five times and take the average value. C.6.4 Drawing of standard curve
Use peak area A as the ordinate and corresponding concentration c (μg/mL) as the abscissa to obtain the standard curve. C.7 Expression of results
Read the concentration of toluene or xylene in the sample solution directly from the standard curve. The toluene or xylene content X in the sample is measured by the sieve formula: X:
Wherein:
X--toluene or xylene content in the sample, in grams per kilogram (g/kg); Ct
The toluene or xylene concentration in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); the volume of the sample solution, in milliliters (mL); the mass of the sample, in grams (g);
-dilution factor.
GB18583—2001
D.1 Scope
Appendix D
(Normative Appendix)
Determination of free toluene diisocyanate content in polyurethane adhesives Gas chromatography
This method is applicable to the determination of free toluene diisocyanate content in polyurethane adhesives for indoor architectural decoration and renovation. This method can determine the polyurethane adhesive for indoor architectural decoration with a free toluene diisocyanate content of more than 0.1g/kg. D.2 Principle
After the sample is diluted with an appropriate solvent, n-tetradecane is added as an internal standard. The diluted sample solution is injected into the injection device and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column, detected and recorded with a hydrogen flame ionization detector, and the chromatogram is calculated by the internal standard method. D.3 Reagents
D.3.1 Ethyl acetate: add 100g 5A molecular sieve (D.3.4), place for 24h and filter; D.3.2 Toluene diisocyanate;
D.3.3 n-tetradecane: chromatographically pure;
D.3.4 5A molecular sieve: heat in a high-temperature furnace at 500C for 2h, place in a desiccator to cool for use. D.4 Instruments
D.4.1 Injection device: 5μL micro-syringe; D.4.2 Chromatography: with hydrogen flame ionization detector; D.4.3 Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; D.4.4 Recording device: integrator or chromatographic workstation; D.4.5 Determination conditions
D.4.5.1 Vaporization chamber temperature: 16 0C;
D.4.5.2 Detection room temperature: 200C;
D.4.5.3 Column box temperature: 135℃;
D.4.5.4 Nitrogen: purity greater than 99.9%, column head pressure 100kPa (135℃); D.4.5.5 Hydrogen: purity greater than 99.9%. Silica gel dehydration, column head pressure 65kPa; D.4.5.6 Air: Silica gel dehydration, column head pressure 55kPa. D.5 Analysis steps
D.5.1 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g toluene diisocyanate in a 50mL volumetric flask, add 5ml internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4966.1 Toluene, m-xylene, p-xylene, o-xylene standard solutions: 1.0 mg/mL, 1.0 mg/mL, 1.0 mg/mL Weigh 0.1000g toluene, 0.1000g m-xylene, p-xylene, 0.1000g o-xylene, place in a 100ml volumetric flask, dilute to scale with ethyl acetate, and shake well. C.6.2 Preparation of series standard solutions
According to the volume of standard solution (B.6.1) listed in Table C.1, add them to six 25mL volumetric flasks respectively, dilute to scale with ethyl acetate, and shake well.
Table C.1 Volume of standard solution (B.6.1) and corresponding concentration Volume transferred
Corresponding toluene concentration
(μg/mL)
C.6.3 Determination of peak area of ​​series of standard solutions Corresponding tom-xylene and
p-xylene concentration
(μg/mL)
Corresponding too-xylene concentration
(μg/mL)
Turn on the gas chromatograph and set the chromatographic conditions. After the baseline is stable, use a 5uL syringe to inject 2uL of standard solution and measure the peak area. Inject each standard solution five times and take the average value. C.6.4 Drawing of standard curve
Use peak area A as the ordinate and corresponding concentration c (μg/mL) as the abscissa to obtain the standard curve. C.7 Expression of results
Read the concentration of toluene or xylene in the sample solution directly from the standard curve. The toluene or xylene content X in the sample is measured by the sieve formula: X:
Wherein:
X--toluene or xylene content in the sample, in grams per kilogram (g/kg); Ct
The toluene or xylene concentration in the sample solution read from the standard curve, in micrograms per milliliter (μg/mL); the volume of the sample solution, in milliliters (mL); the mass of the sample, in grams (g);
-dilution factor.
GB18583—2001
D.1 Scope
Appendix D
(Normative Appendix)
Determination of free toluene diisocyanate content in polyurethane adhesives Gas chromatography
This method is applicable to the determination of free toluene diisocyanate content in polyurethane adhesives for indoor architectural decoration and renovation. This method can determine the polyurethane adhesive for indoor architectural decoration with a free toluene diisocyanate content of more than 0.1g/kg. D.2 Principle
After the sample is diluted with an appropriate solvent, n-tetradecane is added as an internal standard. The diluted sample solution is injected into the injection device and carried into the chromatographic column by the carrier gas. It is separated into corresponding components in the chromatographic column, detected and recorded with a hydrogen flame ionization detector, and the chromatogram is calculated by the internal standard method. D.3 Reagents
D.3.1 Ethyl acetate: add 100g 5A molecular sieve (D.3.4), place for 24h and filter; D.3.2 Toluene diisocyanate;
D.3.3 n-tetradecane: chromatographically pure;
D.3.4 5A molecular sieve: heat in a high-temperature furnace at 500C for 2h, place in a desiccator to cool for use. D.4 Instruments
D.4.1 Injection device: 5μL micro-syringe; D.4.2 Chromatography: with hydrogen flame ionization detector; D.4.3 Chromatographic column: large-bore capillary column: DB-1 (30m×0.53mm×1.5um), the stationary liquid is dimethylpolysiloxane; D.4.4 Recording device: integrator or chromatographic workstation; D.4.5 Determination conditions
D.4.5.1 Vaporization chamber temperature: 16 0C;
D.4.5.2 Detection room temperature: 200C;
D.4.5.3 Column box temperature: 135℃;
D.4.5.4 Nitrogen: purity greater than 99.9%, column head pressure 100kPa (135℃); D.4.5.5 Hydrogen: purity greater than 99.9%. Silica gel dehydration, column head pressure 65kPa; D.4.5.6 Air: Silica gel dehydration, column head pressure 55kPa. D.5 Analysis steps
D.5.1 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g toluene diisocyanate in a 50mL volumetric flask, add 5ml internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4961 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g of toluene diisocyanate in a 50mL volumetric flask, add 5ml of internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 4961 Preparation of internal standard solution
Weigh 1.0006g of n-tetradecane in a 100mL volumetric flask, dilute to scale with dehydrated ethyl acetate, and shake well. D.5.2 Determination of relative mass correction factor
Weigh 0.2g~0.3g of toluene diisocyanate in a 50mL volumetric flask, add 5ml of internal standard, dilute with an appropriate amount of ethyl acetate, take 1L for injection, and determine the chromatographic peak area of ​​toluene diisocyanate and n-tetradecane. Calculate the relative mass correction factor according to the formula. The calculation formula of the relative mass correction factor () is: 496
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