Some standard content:
ICS 71. 040. 30
HG/T2891-1997
Registration No. 427—1997
This standard provides two levels: analytically pure and chemically pure. The analytically pure is equivalent to the ACS (1987) standard "isoamyl alcohol". The differences are as follows. 1 Standard number
According to my country's national conditions, this standard adds three chapters: properties, inspection rules, packaging and marking. 2 Specifications
The analytically pure standard of this standard has three more items than the ACS standard: boiling point, iron, and easily carbonized substances. The four items of evaporation residue, moisture, acidity, acid and ester are stricter than the ACS standard, and the other items are the same as the ACS standard. 3 Test
Except for the determination method of acid and ester, which is consistent with the ACS standard, the other determination methods of this standard refer to the corresponding standards in a set of general test methods for chemical reagents that have been formulated in my country. This set of standards is basically formulated based on IS06353-1:1982 "Chemical Analysis Reagents Part 1: General Test Methods".
This standard is formulated on the basis of ZB/TG63001--1986 "Chemical Reagent Isoamyl Alcohol" standard. Compared with the original standard, the aldehyde and potassium hydroxide tests have been cancelled, and corresponding changes have been made in specifications and test methods. From the date of entry into force, this standard will replace ZB/TG63001--1986. This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Beijing Chemical Reagent General Factory. This standard is drafted by Shanghai Reagent Factory No. 1. The main drafters of this standard are Chen Haoyun and Shen Zhixi. 1195
Chemical Industry Standard of the People's Republic of China
Chemical reagent—Isoamyl alcohol (3-Methyl-1-butanol) Indicative formula: (CH)2CHCHzCH2OH
Relative molecular mass: 88.15
1 Scope
HG/T 2891 --- 1997
This standard specifies the technical requirements, test methods, inspection rules, packaging and marking of the chemical reagent isoamyl alcohol. 2 Reference 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 the 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 (volume analysis) of chemical reagents GB/T 602-—1988
Chemical reagents
Preparation of standard solutions for determination of impurities
GB/T603—1988 Preparation of preparations and products used in test methods for chemical reagents GB/T 606-1988bzxz.net
GB/T 616--1988
GB/T 619--1988
GB/T6682—1992
GB/T9722--1988
GB/T 9733-1988
Chemical reagents
Chemical reagents
Chemical reagents
General method for determination of water content (Karl Fischer method) (eqvISO6353-1:1982)General method for determination of boiling point
Sampling and acceptance rules
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)Chemical reagents
Chemical reagents
GB/T 9736—1988
GB/T 9737--1988
GB/T 9739—1988
GB/T 9740~-1988
GB 15346—1994
3 Properties
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
General principles for gas chromatography
General method for determination of carbon-based compounds (eqvISO6353-1:1982) General method for determination of acidity and alkalinity (eqvISO6353-1:1982) General method for determination of easily carbonizable substances (eqvISO6353-1:1982) General method for determination of iron (eqvISO6353-1:1982) General method for determination of evaporation residue (eqvISO6353-1:1982) Chemical reagents
Packaging and marking
This reagent is a colorless transparent liquid. It has a special odor, is slightly soluble in water, and can be miscible with alcohol, ether, benzene, etc. Density (20℃) is about 0.811 g/mL
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 21, 1997 1196
Implemented on January 1, 1998
Content (C, H120), %
Boiling point (℃)
Evaporation residue, %
Acidity (in terms of H+), mmol/100 g
Acid and ester C in terms of CH.COO(CH,).CH, %, Base compound (in terms of CO), %
Easily carbonizable substances
Iron (Fe), %
Water (H, O), %
5Test
HG/T 2891 -- 1997
130±1
Unless otherwise specified in this chapter, the standard titration solutions, standard solutions, preparations and products used shall be prepared in accordance with GB/T 601--1988, GB/T602-1988 and GB/T603-1988. The water used in the experiments shall conform to the specification of Grade 3 water in GB/T6682-1992. Samples shall be measured accurately to 0.1 mL.
5.1 Content
Determine according to GB/T9722-1988, including: 5.1.1 Determination conditions
Detector: thermal conductivity detector;
Carrier gas and flow rate: hydrogen, 45mL/min, column length (glass column or stainless steel column): 3m; column inner diameter: 3mm;
Stationary phase: 10% polyethylene glycol 20M coated on 101 white silanized carrier [0.18mm~0.25mm (60 days~80 days)], aged at 180℃ for more than 4,
Column temperature: 80℃,
Vaporization chamber temperature: 180℃;
Detection chamber temperature: 180℃;
Injection volume: 4 μL,
Effective plate height of chromatographic column: Het4.8mm;
Asymmetry factor: f≤1.2,
Resolution of difficult-to-separate pairs of substances: R≥1.5 (n-pentanol and isopentanol); Relative retention value of components relative to the main body: r for n-butanol. isopentanol = 0.45; r for n-butanol, isopentanol - 0.64; r for n-butanol, isopentanol = 1.29. 5.1.2 Quantitative method
Determine according to 8.2 of GB/T9722-1988. 5.2 Boiling point
Determine according to GB/T616-1988.
5.3 Evaporation residue
HG/T 2891—1997
Measure 62mL (50g) of chemically pure C and 31mL (25g) of sample, and determine according to GB/T9740-1988. 5.4 Acidity
Determine according to 6.2 of GB/T9736-1988. Wherein: Measure 100mL of carbon dioxide-free water, add 2 drops of phenolic acid indicator solution (10g/L), and use sodium hydroxide standard titration solution (c(NaOH)=0.01mol/L J neutralization, when reaching the end point, the solution is pink, keep it for 30s. Add 25mL (20g) sample, shake in a separatory funnel for 3min, let stand to separate, separate 50mL water phase, add 2 drops of phenolic acid indicator solution (10g/L), titrate with sodium hydroxide standard titration solution Cc (NaOH) = 0.01mol/L) until the solution is pink, and keep it for 30s. The results are calculated according to the provisions of Chapter 7 "Water-insoluble Samples" in GB/T9736--88. 5.5 Acids and esters
5.5.1 Preparation of potassium hydroxide ethanol solution (0.1mol/L) Weigh 7g potassium hydroxide, dissolve in 20mL water, dilute to 1000mL with ethanol, shake, let stand for 24h, and use the clear solution. 5.5.2 Determination method
Measure 62mL (50g) sample, add 50mL isopropanol, add 25.00mL potassium hydroxide ethanol solution (0.1mol/L), heat to reflux in a water bath for 15min, wash the condenser with 20mL carbon dioxide-free water, add 2 drops of phenolic acid indicator solution (10g/L), and titrate with standard hydrochloric acid solution [c(HC1)=0.1 mol/LJ Titrate until the red color of the solution disappears. Perform a blank test at the same time. The mass percentage is calculated according to formula (1):
X(%) = -V:X 130.2 × 100
m × 1 000
Wherein: X is the mass percentage of acid and ester, %; Vi is the volume of the standard hydrochloric acid titration solution in the blank test, mL; V is the volume of the standard hydrochloric acid titration solution, ml.; c is the concentration of the standard hydrochloric acid titration solution, mol/L; - the molar mass of amyl acetate [M(C,H1O,)], g/mol; 130.2—
m—the mass of the sample, g.
5.6 Carbonyl compounds
5.6.1 Preparation of test solution
Measure 2.5 mL (2 g) of sample and dilute it to 100 mL with methanol without carbonyl compounds. 5.6.2 Determination method
Take 1.0mL of test solution and measure it according to the provisions of GB/T9733-1988. The dark red color of the solution shall not be deeper than that of the standard comparison solution. The preparation of the standard comparison solution is to take 0.5mL of test solution and the following amount of carbon-based compound standard solution: analytical pure
chemical pure...
and 1.0mL of test solution at the same time. 5.7 Carbonizable substances
.0.01 mgCO;
?0. 02 mg CO.
Measured according to the provisions of GB/T9737--1988. Among them: 5mL (4.1g) of sample is measured and placed in a 50mL dry colorimetric tube, cooled to 10℃±1℃, and 5mL of 10℃±1℃ sulfuric acid is added dropwise under shaking (the temperature should not exceed 20℃ at this time), and placed in a 10℃±1℃ water bath for 5min. The color of the solution shall not be darker than the following standard colors: analytically pure ·
chemically pure
.·.·H/3 or G/3;
·H/2 or G/2.
Measure 12.3mL (10g) of sample, place it in an evaporating dish, and evaporate it to dryness on a water bath. Dissolve the residue in 1mL hydrochloric acid solution (20%), dilute to 15ml, adjust the pH value of the solution to 2 with ammonia solution (10%), and measure according to GB/T9739-1988. The red color of the solution shall not be darker than the standard comparison solution.
The preparation of the standard comparison solution is to take the following amount of iron standard solution: 1198
HG/T 2891— 1997
Analytical pure
Chemical pure·
-0. 003 mg Fe;
....0. 006 mg Fe.
dilute to 15mL, adjust the pH value of the solution to 2 with hydrochloric acid solution (15%), and treat it in the same way as the adjusted test solution. 5.9 Water
Determine according to GB/T6061988. Among them: measure 5mL (4.1g) sample and use 10mL methanol as solvent. 6 Inspection rules
Sampling and acceptance shall be carried out according to GB/T619—1988. Packaging and marking
Packaging, storage and transportation shall be carried out in accordance with GB15346-1994, and marking shall be given, including: Packaging unit: Class 4 and 5;
Inner packaging form: NB-20.NBY-20, NB-21, NBY-21, NB-26, NBY-26, NB-27, NBY-27, NB-29, NBY-29; Isolation material: GC-2, GC-3
Outer packaging form: WB-1.
The label should indicate "flammable items".
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