This standard specifies the requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial dioctyl phthalate. This standard applies to dioctyl phthalate prepared by esterification of phthalic anhydride and octanol (2-ethylhexyl alcohol). It is mainly used in industries such as plastics, rubber, paints and emulsifiers. GB/T 11406-2001 Industrial dioctyl phthalate GB/T11406-2001 Standard download decompression password: www.bzxz.net

GB/T11406-2001
This standard is a revision of the national standard GB/T11406-1989 "Industrial dioctyl phthalate". The main technical differences between this standard and GB/T11406-1989 are: the two technical indicators "color after heat treatment" and "heating loss" are removed, the technical indicator "water" is added, and the "ester content" is changed to purity".
This standard replaces GB/T11406-1989 from the date of implementation. This standard is proposed by the State Petrochemical Industry Bureau. This standard is under the jurisdiction of the Chemical Additives Sub-Technical Committee of the National Rubber and Rubber Products Standardization Technical Committee. The main drafting unit of this standard: Shandong Qilu Plasticizer Co., Ltd. The main drafters of this standard: Zhou Jianxiu, Li Yan, Han Bangyou, Xing Guangquan This standard was first issued on March 27, 1989 227
National Standard of the People's Republic of China
Di-(2-ethylhexyl)phthalate for industrial use
Di-(2-ethylhexyl)phthalate for industrial use GB/T 11406-—2001
Replaces GB/T11406—1989
Warning: Personnel using this standard should be familiar with formal laboratory operating procedures. This standard does not intend to involve all safety issues that may arise from the use of this standard. It is the user's responsibility to develop appropriate safety and health systems and ensure compliance with national regulations. 1 Scope
This standard specifies the requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial dioctyl phthalate. This standard applies to dioctyl phthalate prepared by esterification of phthalic anhydride and octanol (2-ethylhexanol). It is mainly used in industries such as plastics, rubber, paints and emulsifiers. Molecular formula: C2H3804
Structural formula:
COOCH,CH(CH,);CH
COOCH,CH(CH2);CH3
Relative molecular mass: 390.56 (according to the 1997 international relative atomic mass) 2 Cited standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601-1988 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T603-1988 Preparation of preparations and products used in chemical reagent test methods GB/T 1250--1989
Expression and determination methods of limit values ​​GB/T1664-1995Determination of appearance color of plasticizers GB/T 1672-1988
Determination of volume resistivity of liquid plasticizers
GB/T4472-1984
General rules for determination of density and relative density of chemical products GB/T6489.1~6489.4-2001Testing methods for industrial phthalates GB/T6680-1986General rules for sampling of liquid chemical products GB/T 6682-1992
Specifications and test methods for water used in analytical laboratories (negISO3696:1987) GB/T 8170--1987
Rules for rounding off values
GB/T 11133—1989
Determination of water content in liquid petroleum products (Karl Fischer method) 3 Requirements
3.1 Appearance: Transparent, oily liquid with no visible impurities. Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on 2001-08-28 228
Implementation on 2002-05-01
GB/T 11406—2001Www.bzxZ.net
3.2 Industrial dioctyl phthalate shall comply with the requirements of Table 1. Table 1 Technical indicators of industrial dioctyl phthalate Items
Color, (platinum-cobalt) number
Purity, %
Density (20℃), g/cm3
Acidity (calculated as phthalic acid), %
Water, %
Flash point, ℃
Superior products
Volume resistivity, ×10°α·m
1) According to user needs, the volume resistivity index can be added by negotiation between the supply and demand parties. Test method
Second-class products
0. 982~~0.988
Qualified products
The standard titration solutions, preparations and products used in this standard shall be prepared in accordance with the provisions of GB/T601 and GB/T603 when no other requirements are specified. The test water shall comply with the provisions of GB/T6682 Grade 3 water. 4.1 Determination of chromaticity
The determination shall be carried out in accordance with the provisions of GB/T1664.
4.2 Determination of purity
4.2.1 Principle
Take an appropriate amount of sample and inject it into the gas chromatograph, which is carried into the chromatographic column by the carrier gas for separation. The effluent is detected by the hydrogen flame ionization detector, and the chromatogram is recorded. The purity of dioctyl phthalate is directly calculated by the area normalization method. 4.2.2 Reagents and materials
Carrier gas and auxiliary gas:
a) Nitrogen: purity not less than 99.99%;
b) Hydrogen: purity not less than 99.99%;
c) Compressed air: after purification.
4.2.3 Instruments
4.2.3.1 Gas chromatograph: Detector: hydrogen flame ionization detector. 4.2.3.2 Chromatographic column
a) Quartz capillary column: 0.53mm×15m×0.1μm commercial column, the stationary liquid is phenyl (50%) methyl polysiloxane (0V17).
b) Aging of quartz capillary column: Install the capillary column in the chromatograph column box, check the air tightness, and start nitrogen aging from the column temperature of 100℃. When the temperature rises to 270℃, age for more than 7 hours until the baseline is stable. 4.2.3.3 Injector: 10uL micro glass syringe. 4.2.3.4 Integrator or chromatographic data processor 4.2.4 Operating steps
4.2.4.1 Adjust the instrument according to the following conditions. Appropriate changes are allowed according to different instruments. The appropriate separation degree should be obtained by programmed temperature rise:
a) Initial temperature: 150C;
b) Initial duration: 2min;
c) Heating rate: 10℃/min;
d) Final temperature: 240℃;
e) Final temperature duration: 10min;
f) Vaporization chamber temperature: 260℃;
g) Detection chamber temperature: 260℃;
h) Nitrogen flow rate: 30mL/min;
i) Hydrogen flow rate: 30mL/min;
j) Air flow rate: 300mL/min.
4.2.4.2 Calculation method: Area normalization method. GB/T11406—2001
4.2.4.3 Test: Adjust the instrument according to the above provisions. After the baseline is stable, inject the sample with a micro-syringe and start the integrator or data processor at the same time. The instrument automatically gives the area percentage of each component. If the linear range of the instrument can meet the requirements of the normalization method quantitative analysis and the sample purity is about 98% or more, the purity of dioctyl phthalate can be directly determined. Otherwise, its absolute purity cannot be determined. 4.2.4.4 Chromatogram and relative retention time: The chromatogram is shown in Figure 1. 14
1—2-ethylhexanol; 2—butyric acid octanoic acid; 3—unknown peak; 4—dioctyl ester; 5—benzoic acid; 6—octyl benzoate; 7—unknown peak; 8—dibutyl phthalate; 9—unknown bee; 10—unknown peak, 11—butyl octyl phthalate; 12—unknown peak; 13—diisooctyl phthalate; 14—dioctyl phthalate Figure 1 Chromatogram of industrial dioctyl phthalate 230
Relative retention time is shown in Table 2.
GB/T 11406-2001
Table 2 Relative retention time of each component on the chromatographic column (OV-—17)Peak sequence
4.2.4.5 Expression of analysis results
2-ethylhexanol
Octyl butyrate
Unknown peak
Dioctyl ester
Octyl benzoate
Unknown peak
Dibutyl phthalate
Unknown peak
Unknown peak
Butyl octyl phthalate
Unknown peak
Di-isooctyl phthalate
Dioctyl phthalate
Dioctyl phthalate Content X1, expressed in mass percentage, is calculated according to formula (1): X_
A + ZA,
Where: A-
X (100 - X,),
Peak area of ​​dioctyl phthalate in the sample, mm\, sum of peak areas of all impurities in the sample, mm2; X, — water content in the sample,%.
Relative retention time/min
4.2.5 Allowable difference
The difference between two parallel determination results shall not exceed 0.15%, and the arithmetic mean of the two parallel determination values ​​shall be taken as the purity of the sample. 4.2.6 Detection limit
Minimum detection concentration 0.002%.
4.3 Determination of density
Determine in accordance with the provisions of 2.3.2 Wei's balance method in GB/T4472--1984. 4.4 Determination of acidity
Carry out in accordance with GB/T6489.2-2001.
4.5 Determination of water
Determine in accordance with the provisions of GB/T 11133. 4.6 Determination of flash point
Perform according to GB/T6489.4-2001.
4.7 Determination of volume resistivity
Perform according to the provisions of GB/T1672.
5 Inspection rules
This product shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that all indicators of the products meet the requirements of this standard and shall attach a quality certificate in a certain format in accordance with 5.1
GB/T11406--2001
. The certificate shall include the manufacturer's name, product name, grade, batch number, production date and standard number. 5.2 The receiving unit has the right to inspect and accept the received dioctyl phthalate in accordance with the technical conditions, inspection rules and test methods specified in this standard (the effective quality assurance period is three months from the date of production). 5.3 This product is a batch of individual cans or uniform products packaged at one time. 5.4 Sampling shall be carried out in accordance with the provisions of GB/T6680, and the sampling volume shall not be less than 1000mL. After mixing and evenly hooking, the mixture shall be divided into two clean and dry ground-mouth bottles, and labels shall be affixed to indicate: product name, sampling date, batch number, and sampler. One bottle shall be inspected and the other bottle shall be kept for three months for inspection.
5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling shall be carried out; if it is barrel packaging, sampling shall be carried out from twice the amount of packaging containers for re-inspection. If the results obtained do not meet the requirements of the standard even if only one indicator does not meet the requirements of the standard, the entire batch of products shall be unqualified products. 5.6 When the supply and demand parties have objections to the product quality, the arbitration unit may be selected by negotiation between the two parties and shall be inspected according to the test methods specified in this standard.
6 Marking, packaging, transportation, purchase and storage
6.1 Marking
Each packaging container shall be painted with a mark, including the manufacturer's name, product name, and net content. Each packaging barrel should be affixed with a factory certificate indicating the manufacturer's name, product name, batch number, grade, and packaging date. 6.2 Packaging
Dioctyl phthalate should be packed into a firm, dry, clean 200L galvanized iron or steel barrel. The screw opening of the barrel cover should be sealed with a clean polyethylene or colorless rubber ring to prevent leakage. The product bulk container must also meet the above requirements. 6.3 Transportation and storage
Dioctyl phthalate should be stored in a dry, ventilated warehouse or cargo shed, and violent impact should be avoided during transportation. 232
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