GB/T 6324.3-2011 English PDF (GBT6324.3-2011)

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GB/T 6324.3-2011: Test method of organic chemical products -- Part 3: Determination of permanganate-reducing substances
GB/T 6324.3-2011
Test method of organic chemical products.Part 3. Determination of permanganate-reducing substances
ICS 71.080.01
G15
National Standards of People's Republic of China
Replacing GB/T 6324.3-1993
Test Method for Organic chemical products
Determination of permanganate reducing substances. Part 3
Part 3. Determinationofpermanganate-reducingsubstances
Issued on. 2011-06-16
2011-11-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
GB/T 6324 "Test Methods for Organic Chemical Products" is divided into the following sections.
--- Part 1. Liquid water-miscible organic chemical products test;
--- Part 2. Determination of the volatile organic liquid residue after evaporation of the water bath dry;
--- Part 3. Determination of permanganate reducing substances;
--- Part 4. organic liquid chemicals - Determination of trace sulfur Microcoulomb;
--- Part 5. Determination of organic chemical products of carbonyl compounds content.
This section GB/T 36324 Part of.
This section drafted in accordance with GB/T 1.1-2009 given rules.
This Part replaces GB/T 6324.3-1993 "Determination of organic chemical products potassium permanganate reducing substances", and
GB/T 6324.3-1993 compared to the main technical changes are as follows.
--- Modify the standard name;
--- Modify the preparation of standard solutions used colorimetric reagent (see 3322, 1993 edition of the 3.1.2.2...);
--- Analysis step manner observed by the axial observation amended as seen in the axial or lateral observed (see 334, 1993 edition of the 3.1.2.2..);
--- Deleted recommended some of the products used in the standard colorimetric solution ratio table (see the 1993 edition of the Table A.1).
This section uses redrafted law Reference ASTMD1363. "Test methods of acetone and methanol permanganate time" preparation of 2006,
And ASTMD1363.2006 is non-equivalent.
This part is proposed by the China Petroleum and Chemical Industry Association.
This part of the National Standardization Technical Committee Chemistry Organic Chemicals Branch (SAC/TC63/SC2) centralized.
This section drafted by. China Petroleum and Chemical Corporation Beijing Research Institute of Chemical Industry, China Petrochemical Group of Sichuan Vinylon Works.
Participated in the drafting of this section. Jiangsu SOPO (Group) Co., Ltd., Daqing Oilfield Methanol Plant, China Sinopec Beijing Yanshan Company, Zhejiang
Jin Ju Chemical Co., Ltd. and Shaanxi Yulin Natural Gas Chemical Co., Ltd.
The main drafters of this section. Guo Yanling, Li Po Jun, Zeng Yan.
This section was first released in 1986, in December 1993 the first amendment.
Test Method for Organic chemical products
Determination of permanganate reducing substances. Part 3
1 Scope
This section provides organic chemical products, substances reducing potassium permanganate measured visual colorimetry and titration.
This section applies to visual colorimetry alcohols, ketones and other neutral, weakly acidic and weakly basic organic chemical products potassium permanganate reducing substance test
Set; titration apply potassium permanganate index equal to or greater than 10mg/100mL and does not react with potassium permanganate under acidic conditions
Organic chemical products.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
Preparation of GB/T 601 chemical reagent standard titration solution
GB/T 603 chemical reagent in test methods - Preparations with (GB/T 603-2002, ISO 6353-1. 1982, NEQ)
GB/T 3143 Determination of color liquid chemicals (Hazen unit --- platinum - cobalt color number)
GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)
Test Method 3
3.1 Warning
Some test procedures prescribed test method can lead to dangerous situations, the operator should take appropriate safety and health practices.
3.2 General Provisions
Unless otherwise indicated in the analysis using only recognized as analytical reagents and GB/T 6682 provisions tertiary water.
Used in the analysis standard titration solution, preparations and products, did not indicate when the other requirements, according to GB/T 601, GB/T 603 of Regulation
Set preparation.
3.3 visual colorimetry
3.3.1 Method summary
Under specified conditions, the potassium permanganate solution is added to the sample material can be reacted with potassium permanganate, and be reduced to manganese dioxide, and
Test solution turns from orange pink. Observe and record the time or potassium permanganate pink faded color test solution and standard colorimetric solution
Color coincides with the time the test results are expressed as potassium permanganate time.
1) Preparation of potassium permanganate solution preparation water. take a certain amount of water, adding an appropriate amount of potassium permanganate solution (about 0.2g/L) so that was pale pink, boiled
30min. Such as pale pink disappears, and then supplemented with potassium permanganate solution was pale pink. Cooling to room temperature, the standby.
3.3.2 Reagents
3.3.2.1 potassium permanganate solution. 0.2g/L, 0.2g of potassium permanganate weighed, to the nearest 0.001g, 1) pre-dissolved in treated water, means
Brown in 1000mL volumetric flask, and dilute to the mark. This solution can be stored at room temperature in the dark for two weeks.
3.3.2.2 chloride, cobalt and platinum - cobalt colorimetric standard solution. Weigh 2.00g of cobalt chloride (CoCl2 · 6H2O), with a small amount of water dissolved into
100mL volumetric flask, dilute to the mark. Take 5mL this cobalt chloride solution and adding number 7.5mL500 platinum - cobalt standard solution (in accordance with
The provisions of GB/T 3143 is formulated), transferred to 50mL volumetric flask, dilute to the mark and mix thoroughly. The standard colorimetric solution
Color represents the end color of the test solution fade after the potassium permanganate test.
Cobalt chloride solution and platinum No. 500 - the ratio of cobalt standard solution can be adjusted according to the product standards.
3.3.3 Instruments
3.3.3.1 low temperature water bath. the temperature can be controlled at (15 ± 0.5) ℃ or (25 ± 0.5) ℃.
3.3.3.2 colorimetric tube. 50mL or 100mL (50mL graduated at the line), a colorless transparent glass, with ground glass stopper.
3.3.4 Analysis of step
3.3.4.1 according to product standard sample, placed in a colorimetric tube.
3.3.4.2 will be filled with the sample cuvette is placed in a controlled temperature (15 ± 0.5) ℃ or (25 ± 0.5) ℃ water bath. After 15min from the water
Bath removed colorimetric tube, according to product standards for admission to a predetermined amount of potassium permanganate solution (starting accession recording time), immediately stopper, shake
Uniform, then back into the water bath. Often colorimetric tubes are removed from the water bath, with a white background, lateral or axial observe the color of the test solution or
Comparing the same volume of standard colorimetric solution, if necessary, leaving the background distance 50mm ~ 150mm. Near the measurement result, every minute
Compare bell once, recording test solution pink just fade time or test time color of the solution with the standard colorimetric solution consistent time.
During the experiment the test solution to avoid direct exposure to strong sunlight.
3.3.5 Expression of results
3.3.5.1 potassium permanganate time. pink test solution time or just fade the color of the test solution from the beginning to the solution was added potassium permanganate
Time standard colorimetric solution when the same color, in minutes (min) meter.
3.3.5.2 If the pink test solution remaining deeper than the standard colorimetric color of the solution, the report potassium permanganate time is greater than tmin; if you try
Pink and standard test solution residual color of the solution rather than the color, the report potassium permanganate time is equal tmin; if the remaining test solution
Pink light color standard colorimetric color of the solution, potassium permanganate is reported less than tmin. Here tmin refers to the sample being tested product standards
Index predetermined value.
3.3.5.3 reportable specific potassium permanganate time in min.
3.3.5.4 take two parallel determination results of the arithmetic average of the results of the report. Two parallel determination results of absolute difference. 100min to
The arithmetic mean of 100min or more, no more than the result of these two measurement; next, the result is not more than 5% of these two measurement arithmetic mean
10%.
3.4 Titration
3.4.1 Method summary
Under specified conditions, in acidic medium, the reaction of the sample with an excess of potassium permanganate solution, the remaining potassium permanganate measured by iodometry
the amount. 100mL sample reducing the number of milligrams of potassium permanganate, potassium permanganate is the index.
3.4.2 Reagents
3.4.2.1 sulfuric acid solution. 137.
3.4.2.2 potassium permanganate solution. 1g/L.
3.4.2.3 KI solution. 100g/L.
3.4.2.4 sodium thiosulfate standard titration solution. c (Na2S2O3) = 0.05mol/L.
3.4.2.5 Starch indicator solution. 10g/L.
3.4.3 Instruments
3.4.3.1 low temperature water bath. the temperature can be controlled at (20 ± 0.5) ℃.
3.4.4 Analysis of step
3.4.4.1 according to product standard sample, placed in a sulfuric acid solution containing 50mL bottle of iodine, mix. This iodine bottle immersed temperature
Control in a water bath (20 ± 0.5) ℃, the holding 15min, with a solution of potassium permanganate solution until Buret not fade so far. Together
Into (10 ± 0.05) mL of potassium permanganate solution. Record total volume of potassium permanganate solution is added to a blank test.
3.4.4.2 stoppered and placed in the dark after 40min. This time can be adjusted according to the characteristics of the sample.
3.4.4.3 An excess of potassium iodide solution, titration with sodium thiosulfate standard titration solution, when the solution is pale yellow, add 0.5mL lake
Pink indicator solution and continue titration to the disappearance of the blue, record volume consumption of sodium thiosulfate standard titration solution.
3.4.4.4 measured at the same time, according to the same procedure and determination, with the same volume of water instead of the sample, using the same amount of reagent solution do
Blank test.
3.4.5 Calculation Results
Potassium permanganate index ρ, values in mg/100mL said, according to the formula (1).
ρ =
(V0-V1) cM
V2 ×
100 (1)
Where.
V0 --- blank test consumption of sodium thiosulfate standard titration solution (3.4.2.4) the value of the volume, in milliliters (mL);
V1 --- sample consumption of sodium thiosulfate standard titration solution (3.4.2.4) the value of the volume, in milliliters (mL);
Accurate c --- sodium thiosulfate standard titration solution concentration value in units of moles per liter (mol/L);
M --- potassium permanganate (15KMnO4
) Numerical molar mass in grams per mole (g/mol) (M = 31.61);
Value V2 --- sample volume in milliliters (mL).
The arithmetic average of the results of two parallel determination for reporting results.
Two parallel determination results allowable difference specified by the product standard.