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1C871. 080. 30
Chemical Industry Standard of the People's Republic of China
Organic Chemical Products
(1999）
Published on 1999-06-16
Implemented on 2000-06-01www.bzxz.net
Published by the State Administration of Petroleum and Chemical Industry
Ics 71. D80. 99
No.: 3732-1999
HG/T 2033—1999
This standard is a product of the chemical industry standard HG\2C3391 industrial phthalate cost standard and the main technical differences between it and HG2033 are as follows: the old standard for chloride content in the superior product is less than (.04%), the first-class product less than 0.005% is changed to the superior product less than 0.002%, the first-class product less than 0.003%; the iron index in the inferior product is equal to 2.003%, the inferior product is less than +0.005, the qualified product is less than or equal to .01% to the superior product less than 0.2%, the inferior product is less than or equal to 0.006%, the qualified product is less than or equal to (.05%); the second half index is changed from less than or equal to 1.0% for both the superior and the first-class to less than or equal to .2% for the superior and the first-class The product is small and dry.
This standard shall be implemented from the date of HG/T2033-91. This standard was proposed by the National Technical Committee for Chemical Standardization, and this standard is under the jurisdiction of the Organic Subcommittee of the National Technical Committee for Chemical Standardization. The drafting unit of this standard: Dalian Husui Organic Chemical Co., Ltd. (Dalian No. 1 Organic Chemical) The drafting units participating in this standard: Yizheng Chemical Fiber Kangrun Special Chemicals Co., Ltd., Jiangyang Hongzuo Synthetic Chemical Factory. The drafters of this standard are Cui Dong, Cui Qiyou, Xin Shoumin, and Shi Yushan. This standard is entrusted to the Organic Subcommittee of the National Technical Committee for Chemical Standardization for interpretation, 33
Chemical Industry Standard of the People's Republic of China
Industrial Antimony Acetate
Antioniany Acetate kor industrial wyeHG/T2033—1999
Replacement HG2.33—1
This standard specifies the requirements, test methods, inspection rules and marking, packaging, storage, etc. of industrial acetic acid. This standard is applicable to industrial acetic acid obtained by the reaction of zirconium dioxide and acetic anhydride. The product is mainly used as a catalyst in the production of acetic acid. Molecular formula: CH, 0, Sh
Physical formula: 29R.89 (according to the 1997 International Standard for Relative Atomic Energy) 2 Reference standards
The provisions contained in the following standards become the provisions of this standard through reference in this standard. When this standard was issued, the versions shown were valid. All standards will be revised. The parties who use the standard should discuss the possibility of using the latest version of the following standards, GB/T
503-88
GB/T 60388
1250-89
GR/T6678-86
GB/T667-80
6682-92
3 Requirements
3.1 Appearance, color powder.
Chemical test
Chemical test
Chemical reagents
Preparation of standard solutions for titration analysis (quantitative analysis) Preparation of standard solutions for determination of impurities (NEI50635.3-111982) Preparation of preparations and products used in the test method (AEGS06353-:1982) Methods for expressing and determining reporting limit values General list of chemical product sampling
General rules for sampling of solid chemical products|| tt||Specifications and test methods for water used in analytical laboratories (m-9IS03606:157) Color step method list
The quality of industrial acetic acid rust should meet the requirements of Table 1. Table 1 requires
Combination content, chemical content. And
Recovery content
Hand* content-56
Test method
First-class product
Especially qualified product
G, GOE
The reagents and water used in this standard shall use analytical pure reagents and first-class water specified in Na/T 5582 unless otherwise specified.
National Institute of Chemical Industry Approved on June 16, 1999 Validity date: June 1, 2000
HG/T2Q33-1599
This standard uses standard titration solutions. Standard titration solutions for determination of impurities, preparations and products with other requirements specified shall be prepared in accordance with GB/T601, GB/T502, GB/3.
4.1 Determination of tin content
4.1.1 Method summary
In the test piece, titrate with standard potassium hydroxide solution. The end point is determined by the disappearance of the color of the indicator, and the content is calculated according to the volume of the standard titration solution. 4.1.2 Reagents and solutions
4. 1.2. : Hydrochloric acid solution: -3 + 4.1.2.
4.1-22 Standard titration of acid bomb: r(1/6K:()) 0.1nol/。 4.1.2.3 Single-base control indicator solution: 1g gate: 4..3 Analysis steps
Weigh U.-0.3 sample (accurate to 0.0002s), put it in a 500ml bottle, dissolve 50mL salt solution, add 15=..715 drops of methyl indicator solution, and immediately titrate with potassium standard to determine the concentration. When the red color of the solution gradually weakens, the titration rate changes slowly. When approaching the end point, 1~3 drops of methyl indicator solution should be added until the red color of the solution disappears completely, which is the end point. At the same time, do a blank test:
4.1.4 Analysis results
The mass percentage of the effective content (X) is calculated according to formula (13, X,-(V, V3ex0.u6) 875x100-VV)X6.C875Tre
Calculation:
The sample consumes 100% potassium phosphate standard titration volume, and the empty volume of the standard solution is determined by adjusting the moi/. of the solution; the actual concentration of the solution is estimated by changing the potassium phosphate standard titration filter (moi/.)
The mass of the sieve expressed in grams is equivalent to 1.00ral. Reading potassium standard titration filter c(1/6KBrO,)=:300mul/L7:
The mass of the sample is expressed in grams, points:
4.7.5 Supplementary information
Take the arithmetic half-mean of the results of the two determinations as the determination result, and the difference between the results of two parallel determinations shall not exceed 12%. 4.2 Chloride determination 4.2.1 Reagents and solutions 4.2.1.1 Nitric acid solution, 1-7, 4.2.1-2 Tartaric acid solution: 100 g. 4.2.1.3 Caustic soda solution, 1 mol/L (AgO.). 1 mol/L 4.2.4 Hydride standard solution: 1 mL containing C: mCl-. 4.2.2 Analysis step Sieve Take 1.2 mL of sample (accurate to 1 mL). Add 15 mL of a colorimetric tube, such as 1 mL nitric acid solution and 3 mL silver nitrate solution, dilute to the mark, and place for 5 minutes. Compare with the standard solution. The concentration should not be greater than that of the standard solution.
Standard ratio: Take the oxide standard (superior product is CFmI, qualified product is 0.?m1.), and treat it in the same way as the sample:
4.3 Determination of deficiency
4.3.1 Test and penetration liquid
4.3.1.1 Hot acid solution: 15.
4.3.1.2 Hydrogen peroxide solution: 1 ten!
4.3.1.3 Thiosulfate solution: 1CC/L.
4.3.1.4 Alcoholic acid solution: 1CC/L. HGT20331999
4.3.1.5 Rapid standard solution 1ml. Drop solution contains 0.1mgFe, 4.3.2 Analysis steps
Pipette 0.28 ml (accurate to .), put into a test tube. Add 1n tartaric acid solution to dissolve, add 1 drop and 1m chemistry solution to heat to 100%, cool to 100% and add 5ml. Mix 1ml of the solution, add water to 50% and mix. The color should not be darker than the standard colorimetric solution. Take the standard drop solution (0.4ml for the standard product, 0.8ml for the qualified product) and process it in the same way as the sample.
4.4 Dissociation test
4.4.1 Reagents
Ethylene glycol
4.4.2. Analytical steps
Weigh 0.36% of the sample (accurate to 0.07), put it into a 25ml colorimetric tube, add 2ml of ethylene glycol, stir thoroughly until the sample is dissolved, and measure it every 24 hours. It should be a clear liquid with a bright color. 4.5 Determination of monobenzene
4.5.1 Method Summary
Under certain conditions, the sample is passed through a chromatographic column, and each impurity is separated and detected by an amplified ion detector: Quantification by external standard method: 4.5.2 Reagents and Materials
4.5.2.1 Methane: chromatographically pure,
4.5.2.2 Formaldehyde, without formaldehyde.
4.5-2.3 Carrier gas: nitrogen, purity less than 79.2%, 4.5.2.4 Support gas, organic matter density equal to 99.8%; compressed,
4.5.2.5 Dielectric: 6201, u.2:1-).2mm. 4.5.2.6 Fixed gas: organic electrochemical and ortho-extractive: formic acid main enzyme, 4.5.3 Instruments and equipment
4.5.3.1 The performance of the chromatographic control device of the flame rate detector shall comply with the provisions of Chapter 5 of GB/T 9722-88: 4.5-3.2 Chromatographic column:
4.5.3.2.1 # tube: non-sintering tube, k3m, inner diameter 4mm4.5.3-2.2 The ratio of the medium to the fixed gas is 520:1, organic solvent: 1:1, phthalate: 1:3:25. 4.5.3.2.3 Preparation of chromatographic column: According to GB/T 9722-28. Organic benzoate is dissolved in acetone, the two liquids are combined and separated, and then 6201 carrier is placed in it, and the color injection is filled with about 6g/. Aging at 12℃ for more than 2h
4.5.3.3 Micro or sample injection, 10pl.
4.5.3. Recorder or microprocessor:
4.5. Preparation of standard sample and test rod
Cup sample preparation: weigh the pan to mix the single extractable benzene standard sample, and its concentration should be close to the concentration of the test. Sample preparation: weigh 1 sample (with a total of 0.0002g) and place it in a 10ml container bottle, add: m. Fill, start, and stir for 1min. Set aside.
4.5.5 Chromatography operating conditions
H.:10 mL/mint
N::40 nL/mir.;
Air:103mi/min:
Dust:
Detection temperature:1802;
Vaporization temperature
Injection volume:1-~5 u1.:
4.5.6 Analysis steps
HC/T2033—1999
The instrument was operated according to the instruction manual. The recommended operating parameters are shown in 4.5.5. Sample injection shall be started after the necessary line is stable. Before and after the annual analysis of the sample, the monthly standard sample is positively calibrated with an external standard. The sampling frequency is more than two times, and the arithmetic average of the area is taken as A1. Ar1-;C; 12 to 3- is not used
Figure 1 Typical color disappearance diagram of methyl methacrylate in the industry
4.5.7 Table of analysis results
The content of methyl methacrylate expressed as a percentage of mass
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