Industrial antimony acetate (3)

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Under specified conditions, the sample passes through the chromatographic column, and the impurities are separated and detected by a flame ionization detector

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The performance of the instrument should comply with the provisions of Chapter 5 in GB/T9722-1988

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3 Preparation and aging of the chromatographic column: according to 7.
1 of GB/T9722-1988
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The organic bentonite was dissolved with benzene, and the dinonyl phthalate was dissolved with ether .
The two solutions were combined and mixed, and then the 6201 carrier was poured into it
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The packing volume of the chromatographic column is about 6g/m
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The chromatographic column is aged at 80°C for 2h and at 120°C for more than 2h
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3 Micro sampler: 10uL
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4 Recorder or microprocessor
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4 Preparation of standard samples and test specimens

Preparation of standard sample: Toluene-benzene standard sample prepared by weighing method, its concentration should be close to the concentration of the tested sample
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Sample preparation: Weigh 1g sample (accurate to 0.
0002g), place it in a 10mL volumetric flask, add 5mL benzene, mix well, let it stand for 10min, and set aside
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5 Chromatographic operating conditions

H ₂ : 40mL/min;

N ₂ : 40mL/min;

Air: 400mL/min;

Column temperature: about 90℃;

Inspection temperature: 180℃;

Vaporization temperature: 200℃;

Injection volume: 1μL～5uL
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6 Analysis steps

The operation of the instrument is carried out in accordance with the instruction manual.
The recommended operating conditions are shown in 4.
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5, and the typical chromatogram is shown in Figure 1
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The sample can be injected after the baseline of the instrument is stable
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Before and after each analysis of the sample, the standard sample is used for external standard calibration
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More than twice the number of injections, the arithmetic average of the peak area A _.
1 , A _E
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Figure 1 Typical chromatogram of toluene in industrial acetic acid brocade

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7 Expression of analysis results

The toluene content (X ₂ ) expressed in mass percentage is calculated according to formula (2):

In the formula: the mass of toluene in E ₁ —5mL standard sample, g;

A ₁ —the peak area of ​​toluene in the sample;

A _E —the peak area of ​​toluene in the standard sample;

m—the mass of the sample, g
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8 Tolerance

Take the arithmetic mean of the two parallel determination results as the determination result
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The difference between the two parallel determination results shall not be greater than 0.
04%
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5 Inspection rules

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1 This product should be inspected by the quality inspection department of the manufacturer
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The manufacturer shall ensure that the products manufactured are in compliance with the requirements of this standard, and shall be accompanied by a quality certificate, which includes: the name of the manufacturer, site, product name, grade, batch number, net content, production date and serial number of this standard
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2 Take products of the same quality as a batch, and each batch of products shall not exceed 1000kg
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3 Determine the number of sampling units according to 6.
6 of GB/T6678-1986
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Sampling should meet the requirements of Chapter 2 in GB/T6679-1986
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The sampling volume of each batch shall not be less than 250g
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Mix the sample carefully and put it into a clean and dry ground bottle
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Bottles are labeled with stating: manufacturer name, product name, batch number, date of sampling and so on
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One bottle is used for inspection, and the other bottle is kept for three months for future reference
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4 The test result is judged according to the rounding value comparison method in GB/T1250
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If one of the inspection results does not meet the requirements of the standard, samples should be taken from twice the amount of packaging for re-inspection
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Even if only one index does not meet the requirements of this standard in the re-inspection result, the whole batch of products is unqualified
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6 Marking, packaging, transportation and storage

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1 The packaging container should be painted with firm and obvious signs, indicating: manufacturer name, product name, batch number, trademark, production date, and net content
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2 Industrial antimony acetate is packaged in a dry and clean airtight plastic barrel, with a net content of 12.
5kg per barrel
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3 During transportation, it should be lightly loaded and unloaded, avoiding collisions, and preventing sunlight, rain and moisture
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4 Industrial antimony acetate should be stored in a ventilated, cool and dry place, and the storage period is half a year
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