GB/T 27563-2011 PDF English
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| GB/T 27563-2011 | English | 155 |
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N-Methyl-2-Pyrrolidone for industrial use
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GB/T 27563-2011: N-Methyl-2-Pyrrolidone for industrial use---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT27563-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.40
G 17
N-Methyl-2-Pyrrolidone for industrial use
Issued on: DECEMBER 05, 2011
Implemented on: MAY 01, 2012
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Requirements... 5
4 Test methods... 5
5 Inspection rules... 10
6 Marking, packaging, transportation and storage... 11
Annex A (normative) Typical chromatogram, relative retention value, and relative
correction factor for N-methyl-2-pyrrolidone content determination... 12
N-Methyl-2-Pyrrolidone for industrial use
1 Scope
This Standard specifies the requirements, test methods, inspection rules, as well as
marking, packaging, transportation and storage of N-methyl-2-pyrrolidone for
industrial use.
This Standard applies to N-methyl-2-pyrrolidone synthesized from γ-butyrolactone and
methylamine.
Chemical formula.C5H9ON
Structural formula.
Relative molecular mass. 99.13 (according to the 2007 international relative atomic
mass)
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 325.1, Zinc-coated steel wire ropes for high-pressure rubber hose
GB/T 601, Chemical reagent -- Preparations of reference titration solutions
GB/T 3143, Color determination method of liquid chemicals (Hazen unit - Platinum-
cobalt scale)
GB/T 6283-2008, Chemical products -- Determination of water Karl-Fischer
method (general method) (ISO 760.1978, NEQ)
GB/T 6488, Liquid chemicals -- Determination of refractive index at 20°C
GB/T 6678, General principles for sampling chemical products
GB/T 6680, General rules for sampling liquid chemical products
GB/T 6682, Water for analytical laboratory use -- Specification and test methods
(GB/T 6682-2008, ISO 3696.1987, MOD)
GB/T 8170, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 9722, Chemical reagent -- General rules for the gas chromatography
GB/T 9724-2007, Chemical reagent -- General rule for the determination of pH (ISO
6353-1.1982, NEQ)
GB/T 9725-2007, Chemical reagent -- General rule for potentiometric titration (ISO
6353-1.1982, NEQ)
3 Requirements
3.1 Appearance
It is a colorless or slightly yellow transparent liquid at room temperature.
3.2 Requirements
N-methyl-2-pyrrolidone for industrial use shall meet the technical requirements shown
in Table 1.
4 Test methods
4.1 Warning
Some test procedures specified in the test method may lead to dangerous situations.
Operators shall take appropriate safety and protective measures.
4.2 General provisions
Unless otherwise specified, only analytically pure reagents and grade 3 water as
specified in GB/T 6682 are used in the analyses.
Unless otherwise specified, the standard titration solutions used in the analysis shall be
prepared in accordance with the provisions of GB/T 601.
4.3 Appearance
Take an appropriate amount of laboratory sample into a colorimetric tube. Observe
visually under natural light.
4.4 Determination of N-methyl-2-pyrrolidone content
4.4.1 Method summary
Gas chromatography is used. Under selected chromatographic conditions, the specimen
is vaporized and passed through a capillary column to separate the components.
Detection is by flame ionization detection (FID). Quantification is performed using the
corrected area normalization method. After subtracting water and total amines, the N-
methyl-2-pyrrolidone content is calculated.
4.4.2 Reagents
4.4.2.1 Nitrogen. volume fraction ≥ 99.995%.
4.4.2.2 Hydrogen. volume fraction ≥ 99.99%.
4.4.2.3 Air. purified with activated carbon and blue silica gel, then dried.
4.4.2.4 N-methyl-2-pyrrolidone. chromatographically pure.
4.4.2.5 γ-Butyrolactone. chromatographically pure.
4.4.2.6 1,4-Butanediol. chromatographically pure.
4.4.2.7 2-Pyrrolidone. chromatographically pure.
4.4.3 Instruments
4.4.3.1 Gas chromatograph. equipped with a flame ionization detector (FID). The
sensitivity and stability of the instrument shall comply with the requirements of GB/T
9722.The linear range shall meet analytical requirements.
4.4.3.2 Data processing system. chromatography data processor or chromatography
workstation.
4.4.3.3 Sample injector. 1.0 μL micro syringe or automatic sample injector.
4.4.4 Chromatographic analysis conditions
4.5 Determination of moisture
The determination shall be carried out in accordance with the provisions of Chapter 8
of GB/T 6283-2008.
The arithmetic mean of the two parallel determination results shall be reported as the
result. The absolute difference between the two parallel determination results shall not
exceed 0.003%.
4.6 Determination of chromaticity
The determination shall be carried out in accordance with the provisions of GB/T 3143.
4.7 Determination of refractive index
The determination shall be carried out in accordance with the provisions of GB/T 6488.
4.8 Determination of total amine content
4.8.1 Method summary
Dissolve the sample in isopropyl alcohol. Titrate the alkaline substances in the specimen
with a standard hydrochloric acid solution. Use a potentiometer or pH meter to indicate
the titration endpoint. The total amine content is calculated as monomethylamine.
4.8.2 Reagents
4.8.2.1 Isopropyl alcohol.
4.8.2.2 Standard hydrochloric acid titration solution. c(HCl) = 0.02 mol/L.
4.8.3 Instruments
4.8.3.1 Potentiometer. the accuracy of the potentiometer is ±0.01 mV.
4.8.3.2 Acidity meter. the accuracy of the acidity meter is pH ± 0.01, with temperature
compensation function.
4.8.4 Analysis steps
Weigh 65 g of laboratory sample to the nearest 0.01 g. Place in a 250 mL beaker.
Dissolve in 100 mL of isopropyl alcohol. Shake well. Perform the following
determination according to Chapter 6 of GB/T 9725-2007.
4.8.5 Result calculation
The total amine content is expressed as the mass fraction w2 of monomethylamine
(CH3NH2), expressed in %, and calculated according to formula (3).
Where,
V - the volume of the standard hydrochloric acid titrant (4.8.2.3) consumed by the test
material, in milliliters (mL);
c - the exact concentration of the standard hydrochloric acid titrant, in moles per liter
(mol/L);
m - the mass of the test material, in grams (g);
M - the molar mass of monomethylamine (CH3NH2), in grams per mole (g/mol) (M =
31.06).
The arithmetic mean of the two parallel determination results shall be reported as the
result. The absolute difference between the two parallel determination results shall not
exceed 0.001%.
4.9 Determination of pH
Use a pipette to transfer 10.0 mL of the sample to a 100 mL volumetric flask. Dilute to
the mark with carbon dioxide-free water. Shake well and transfer to a beaker. The
following steps shall be performed in accordance with Chapter 6 of GB/T 9724-2007.
5 Inspection rules
5.1 All items specified in 3.1 and 3.2 Table 1 of Chapter 3 are exit-factory inspection
items. Exit-factory inspection shall be carried out on each batch.
5.2 N-methyl-2-pyrrolidone for industrial use is shipped in batches based on the
quantity of one storage tank or tank truck (ship), or products of equivalent mass.
5.3 The sampling method and number of sampling units for N-methyl-2-pyrrolidone
for industrial use shall comply with the requirements of GB/T 6678 and GB/T 6680.
The sampling volume shall be no less than 400 mL. Divide the sample into two clean,
dry glass bottles and seal them tightly. Label each bottle with the product name, batch
number or production date, sampling date, sampling location, and the name of the
sampler. One bottle shall be used for testing, and the other bottle shall be retained for
future reference.
5.4 N-methyl-2-pyrrolidone for industrial use shall be inspected by the manufacturer's
quality supervision and inspection department. The manufacturer must ensure that each
batch of product meets the requirements of this Standard. Each batch of product must
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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