預(yù)分離柱

固定相：活性炭，粒徑0. 17-0.25 mm(60-80目)

柱管：不銹鋼，長(zhǎng)1m，內(nèi)徑4mm。
型號(hào)：HH-Act carbon

分離柱
固定相:5?分子篩(色譜用)，粒徑 。. 17-0.25 mm (60-80目)。
柱管 不銹鋼，長(zhǎng) 2m，內(nèi)徑 4 mm,
柱溫:15-25 °C，恒定在士1 °c或一78°C

應(yīng)用：GB/T 6022-2008 工業(yè)用丁二烯液上氣相中氧的測(cè)定

GB/T 6022-1999 工業(yè)用丁二烯液上氣相中氧的測(cè)定氣相色譜法

GB/T 6022-1985 工業(yè)用丁二烯液上氣相中氧的測(cè)定 氣相色譜法

1 范圍

1.1本標(biāo)準(zhǔn)規(guī)定了測(cè)定工業(yè)用丁二烯液上氣相中氧含量的氣相色譜法和薄膜覆蓋電池電化學(xué)法，氣相色譜法測(cè)定范圍為100mL/m～5000mL/m，薄膜覆蓋電池電化學(xué)法測(cè)定范圍為1mL/m³～5000mL/m³。

1.2 本標(biāo)準(zhǔn)并沒(méi)有說(shuō)明與使用有關(guān)的所有安全問(wèn)題。因此，使用者有責(zé)任采取適當(dāng)?shù)陌踩c健康措施，符合國(guó)家有關(guān)法規(guī)的規(guī)定。

2 規(guī)范性引用文件

下列文件中的條款通過(guò)本標(biāo)準(zhǔn)的引用而成為本標(biāo)準(zhǔn)的條款。凡是注日期的引用文件，其隨后所有的修改單(不包括勘誤的內(nèi)容)或修訂版均不適用于本標(biāo)準(zhǔn)，然而，鼓勵(lì)根據(jù)本標(biāo)準(zhǔn)達(dá)成協(xié)議的各方研究可使用這些文件的新版本。凡是不注口期的引用文件，其新版本適用于本標(biāo)準(zhǔn)。

GB/T3723工業(yè)用化學(xué)產(chǎn)品采樣安全通則(GB/T3723-1999，idt ISO 3165：1976

GB/T6681氣體化工產(chǎn)品采樣通則

GB/T8170數(shù)值修約規(guī)則

3 氣相色譜法

3.1 方法概要

氣體試樣通過(guò)進(jìn)樣裝置注入色譜儀，并被載氣帶入預(yù)分離柱，烴類(lèi)分被預(yù)分離柱吸附后，反吹預(yù)分離柱，將烴類(lèi)組分放空。其余組分進(jìn)入分離欄分離，用熱導(dǎo)檢測(cè)器檢測(cè)。由丁在環(huán)境溫度下氧與氬在分離柱上不被分離，因此采用氬氣作載氣，使樣品中的氬在熱導(dǎo)池上不產(chǎn)生響應(yīng)。將得到的氧色譜峰面積與從標(biāo)準(zhǔn)樣品得到的氧色譜峰面積相比較，從而測(cè)定試樣中的氧含量。

3.2 試劑和材料

3.2.1 載氣

氬氣：純度不小于99.99%(體積分?jǐn)?shù))，氧含量不大于0.002%(體積分?jǐn)?shù))，不含有機(jī)雜質(zhì)、水及二氧化碳。

3.2.2 制備標(biāo)準(zhǔn)樣品用氣體

氮?dú)饣驓鍤猓杭兌炔恍∮?9.999%(體積分?jǐn)?shù))，氧含量不大于2mL/m.

氧氣：純度不小于99.99%(體積分?jǐn)?shù))。

3.2.3 系列氧標(biāo)準(zhǔn)氣：氧含量為50mL/m～5000mL/m，底氣為氮?dú)饣驓鍤?3.2.2)。

3.2.4 色譜柱固定相

活性炭(色譜用)：粒徑0.17mm～0.25mm(60目～80目)；

5A分子篩(色譜用)：粒徑0.17mm～0.25mm(60目～80目)。

3.3 儀器和設(shè)備

3.3.1 氣相色譜儀：具有氣體定量進(jìn)樣裝置、反吹裝置及熱導(dǎo)檢測(cè)器的氣相色譜儀，該儀器在本標(biāo)準(zhǔn)給定的操作條件下產(chǎn)生的峰高，少要大于儀器噪聲的兩倍、

3.3.2 定量管：1mL或5mL。

3.3.3 預(yù)分離柱

固定相：活性炭(3.2.4)；

柱管：不銹鋼，長(zhǎng)1m，內(nèi)徑4mm。

3.3.4 分離柱

固定：5A分子篩(3.2.4)；

柱管：不銹鋼，長(zhǎng)2m，內(nèi)徑4mm；

5A分子篩的活化：將5A分子篩用蒸餾水洗滌去塵，置入烘箱加熱120℃，恒溫4h，裝柱。在氬氣流下(約100mL/min)將分離柱升溫310℃～320℃，恒溫1h～4h，以除去水、二氧化碳及痕量有機(jī)物?；罨瘯r(shí)間取決于分子篩吸濕量。

3.3.5 記錄裝置：電子積分儀或色譜工作站。

3.3.6 氣體進(jìn)樣閥.

3.3.7 反吹裝置：六通閥。

3.4 采樣

按照GB/T3723和GB/T6681規(guī)定的方法采取丁二烯液上氣相樣品。

工業(yè)用丁二烯液上氣相中氧的測(cè)定5?填充柱 測(cè)試譜圖：



Determination of Oxygen in Industrial Butadiene Over-Liquid Gas Phase 5A Packed Column
Determination of Oxygen in the Gas Phase Over Liquid Butadiene for Industrial Use 5A Packed Column Details:

Pre-separation column

Stationary phase: activated carbon, particle size 0.17-0.25 mm (60-80 mesh)

Column tube: stainless steel, 1m long, 4mm inner diameter.
Model: HH-Act carbon



Separation column
Stationary phase: 5A molecular sieve (for chromatography), particle size . . 17-0.25 mm (60-80 mesh).
Column tube Stainless steel, 2m long, 4mm inner diameter,
Column temperature: 15-25 °C, constant at ±1 °C or -78 °C



Application: GB/T 6022-2008 Determination of oxygen in gas phase above liquid butadiene for industrial use

GB/T 6022-1999 Determination of oxygen in the gas phase above liquid butadiene for industrial use by gas chromatography

GB/T 6022-1985 Determination of oxygen in industrial butadiene liquid over gas phase-Gas chromatography

1 Scope

1.1 This standard specifies the gas chromatography method and the film-covered cell electrochemical method for the determination of the oxygen content in the gas phase of the industrial butadiene liquid. The range is 1mL/m3～5000mL/m3.

1.2 This standard does not address all safety issues related to use. Therefore, it is the user's responsibility to take appropriate safety and health measures to ensure compliance with the relevant national regulations.

2 Normative references

The clauses in the following documents become clauses of this standard through reference in this standard. For dated references, all subsequent amendments (excluding errata content) or revisions do not apply to this standard. However, parties to agreements based on this standard are encouraged to study the latest versions of these documents. For referenced documents with no notation period, the latest editions of them apply to this standard.

GB/T3723 Industrial Chemical Products Sampling Safety General Rules (GB/T3723-1999, idt ISO 3165:1976

GB/T6681 General rules for sampling of gas chemical products

GB/T8170 Numerical Rounding Rules

3 Gas chromatography

3.1 Method overview

The gas sample is injected into the chromatograph through the sampling device, and is carried into the pre-separation column by the carrier gas. After the hydrocarbons are adsorbed by the pre-separation column, the pre-separation column is backflushed to vent the hydrocarbon components. The rest of the components enter the separation column for separation and are detected with a thermal conductivity detector. Since oxygen and argon are not separated on the separation column at ambient temperature, argon is used as the carrier gas, so that the argon in the sample does not respond on the thermal conductivity cell. The oxygen content in the sample was determined by comparing the obtained oxygen chromatographic peak area with the oxygen chromatographic peak area obtained from the standard sample.

3.2 Reagents and materials

3.2.1 Carrier gas

Argon: the purity is not less than 99.99% (volume fraction), the oxygen content is not more than 0.002% (volume fraction), and does not contain organic impurities, water and carbon dioxide.

3.2.2 Gases for preparing standard samples

Nitrogen or argon: the purity is not less than 99.999% (volume fraction), and the oxygen content is not more than 2mL/m.

Oxygen: the purity is not less than 99.99% (volume fraction).

3.2.3 Series of oxygen standard gas: the oxygen content is 50mL/m~5000mL/m, and the bottom gas is nitrogen or argon (3.2.2).

3.2.4 Column stationary phase

Activated carbon (for chromatography): particle size 0.17mm～0.25mm (60 mesh～80 mesh);

5A molecular sieve (for chromatography): particle size of 0.17mm to 0.25mm (60 mesh to 80 mesh).

3.3 Instruments and equipment

3.3.1 Gas chromatograph: a gas chromatograph equipped with a gas quantitative sampling device, a backflushing device and a thermal conductivity detector. The peak height generated by the instrument under the operating conditions given in this standard shall be at least two times greater than the instrument noise. times,

3.3.2 Quantitative tube: 1mL or 5mL.

3.3.3 Pre-separation column

Stationary phase: activated carbon (3.2.4);

Column tube: stainless steel, 1m long, 4mm inner diameter.

3.3.4 Separation column

Fixed: 5A molecular sieve (3.2.4);

Column tube: stainless steel, 2m long, 4mm inner diameter;

Activation of 5A molecular sieve: The 5A molecular sieve was washed with distilled water to remove dust, placed in an oven, heated to 120°C, kept at a constant temperature for 4 hours, and then packed into a column. Under the argon flow (about 100mL/min), the separation column was heated to 310℃～320℃, and the temperature was kept constant for 1h～4h to remove water, carbon dioxide and trace organics. The activation time depends on the amount of moisture absorbed by the molecular sieve.

3.3.5 Recording device: electronic integrator or chromatography workstation.

3.3.6 Gas injection valve.

3.3.7 Backflushing device: six-way valve.

3.4 Sampling

According to the methods specified in GB/T3723 and GB/T6681, the gas phase samples above the liquid of butadiene were taken.




Determination of Oxygen in the Gas Phase on Industrial Butadiene Liquid 5A Packed Column Test Spectrum: