2m*4mm 工业用丁二烯液上气相中氧的测定5Å填充柱

工业用丁二烯液上气相中氧的测定5Å填充柱，室内空气，焦炉煤气，炼厂气，天然气，变压器油，多氯联苯，植物油，增塑剂，塑化剂，消毒剂，氨水，氨气，过氧化物，MTBE，裂解进样器

浩瀚色谱（山东）应用技术开发有限公司(原滕州市浩瀚色谱仪器技术服务有限公司）,是齐鲁大地一家从事色谱仪器技术开发，技术推广的技术型企业，研发出多款新型产品。（一）专用色谱柱：1.氯乙suan直接进样分析专用柱2.氯化氢直接进样分析专用柱3.氯QI直接进样分析专用柱4.四氟化硅直接进样分析专用柱5.六氟二甲基硅醚分析专用柱6.氨气直接进样分析专用柱（二）痕量分析专用气相色谱仪：1.高纯气体中痕量水（ppb级）分析专用气相色谱仪2.纯苯中痕量噻吩（ppb级）分析专用气相色谱仪（三）防腐型气相色谱仪，并成功应用于氟气，氟化氢，氯QI，氨气，酰氯，氯化氢，三氯氢硅，四氟化硅，氯YI酸，氯HUA亚砜，硫化物，二氯化硫等腐蚀性物质检测，产品遍布各个行业及地区，其中不乏有大型央企---中石油，中储粮，秦山核电站，中纺集团等，部分出口。

公司主要业务

1.通用气相色谱仪生产销售：氢火焰检测器气相色谱仪，热导检测器气相色谱仪，火焰光度检测器气相色谱仪，氮磷检测器气相色谱仪，电子捕获检测器气相色谱仪。

2.便携式气相色谱仪，在线气相色谱仪生产销售。

3.专用气相色谱仪研发制造：氧化锆检测器气相色谱仪，氦离子检测器气相色谱仪，氩离子检测器气相色谱仪等。

4.防腐气相色谱仪

5.二维，多维气相色谱仪

6.高效液相色谱仪

7.实验室纯水机，顶空进样器，自动进样器，热解析仪，氮氢空发生器，色谱耗材（色谱柱，石墨垫，稳压阀，压盖钳，顶空瓶，7725进样阀等），分光光度计，电子天平，水分测定仪，干燥箱，离心机，玻璃仪器，化学试剂等整套实验室设备生产销售。

8.提供技术转让，建立分析方法。

9.从事旧色谱以旧换新的业务。

10.色谱柱研制，定做。

11.承接样品的检测业务。

12.承接国内外色谱仪器的维修，改装业务。

浩瀚色谱（山东）应用技术开发有限公司，以客户为中心，想客户所想，销售的不仅仅是产品，重要的是帮助客户解决问题，架起心灵沟通的桥梁。

工业用丁二烯液上气相中氧的测定5Å填充柱
工业用丁二烯液上气相中氧的测定5Å填充柱 详细信息：

预分离柱

固定相：活性炭，粒径0. 17-0.25 mm(60-80目)

柱管：不锈钢，长1m，内径4mm。
型号：HH-Act carbon

分离柱
固定相:5Å分子筛(色谱用)，粒径 。. 17-0.25 mm (60-80目)。
柱管 不锈钢，长 2m，内径 4 mm,
柱温:15-25 °C，恒定在士1 °c或一78°C

应用：GB/T 6022-2008 工业用丁二烯液上气相中氧的测定

GB/T 6022-1999 工业用丁二烯液上气相中氧的测定气相色谱法

GB/T 6022-1985 工业用丁二烯液上气相中氧的测定 气相色谱法

1 范围

1.1本标准规定了测定工业用丁二烯液上气相中氧含量的气相色谱法和薄膜覆盖电池电化学法，气相色谱法测定范围为100mL/m～5000mL/m，薄膜覆盖电池电化学法测定范围为1mL/m³～5000mL/m³。

1.2 本标准并没有说明与使用有关的所有安全问题。因此，使用者有责任采取适当的安全与健康措施，符合国家有关法规的规定。

2 规范性引用文件

下列文件中的条款通过本标准的引用而成为本标准的条款。凡是注日期的引用文件，其随后所有的修改单(不包括勘误的内容)或修订版均不适用于本标准，然而，鼓励根据本标准达成协议的各方研究可使用这些文件的新版本。凡是不注口期的引用文件，其新版本适用于本标准。

GB/T3723工业用化学产品采样安全通则(GB/T3723-1999，idt ISO 3165：1976

GB/T6681气体化工产品采样通则

GB/T8170数值修约规则

3 气相色谱法

3.1 方法概要

气体试样通过进样装置注入色谱仪，并被载气带入预分离柱，烃类分被预分离柱吸附后，反吹预分离柱，将烃类组分放空。其余组分进入分离栏分离，用热导检测器检测。由丁在环境温度下氧与氩在分离柱上不被分离，因此采用氩气作载气，使样品中的氩在热导池上不产生响应。将得到的氧色谱峰面积与从标准样品得到的氧色谱峰面积相比较，从而测定试样中的氧含量。

3.2 试剂和材料

3.2.1 载气

氩气：纯度不小于99.99%(体积分数)，氧含量不大于0.002%(体积分数)，不含有机杂质、水及二氧化碳。

3.2.2 制备标准样品用气体

氮气或氩气：纯度不小于99.999%(体积分数)，氧含量不大于2mL/m.

氧气：纯度不小于99.99%(体积分数)。

3.2.3 系列氧标准气：氧含量为50mL/m～5000mL/m，底气为氮气或氩气(3.2.2)。

3.2.4 色谱柱固定相

活性炭(色谱用)：粒径0.17mm～0.25mm(60目～80目)；

5A分子筛(色谱用)：粒径0.17mm～0.25mm(60目～80目)。

3.3 仪器和设备

3.3.1 气相色谱仪：具有气体定量进样装置、反吹装置及热导检测器的气相色谱仪，该仪器在本标准给定的操作条件下产生的峰高，少要大于仪器噪声的两倍、

3.3.2 定量管：1mL或5mL。

3.3.3 预分离柱

固定相：活性炭(3.2.4)；

柱管：不锈钢，长1m，内径4mm。

3.3.4 分离柱

固定：5A分子筛(3.2.4)；

柱管：不锈钢，长2m，内径4mm；

5A分子筛的活化：将5A分子筛用蒸馏水洗涤去尘，置入烘箱加热120℃，恒温4h，装柱。在氩气流下(约100mL/min)将分离柱升温310℃～320℃，恒温1h～4h，以除去水、二氧化碳及痕量有机物。活化时间取决于分子筛吸湿量。

3.3.5 记录装置：电子积分仪或色谱工作站。

3.3.6 气体进样阀.

3.3.7 反吹装置：六通阀。

3.4 采样

按照GB/T3723和GB/T6681规定的方法采取丁二烯液上气相样品。

工业用丁二烯液上气相中氧的测定5Å填充柱 测试谱图：



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:

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