Method for measuring content of bromide ions in brine by gas chromatography

A gas chromatography, salt brine technology, applied in measurement devices, material separation, instruments, etc., can solve the problems of low accuracy and sensitivity, demanding conditions, complicated operations, etc., and achieve low price, low impurity interference, and good selectivity. Effect

CN103472169AInactive Publication Date: 2013-12-25GUIZHOU NORMAL UNIVERSITY
0 Cites 2 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2013-12-25
Estimated Expiration
Not applicable · inactive patent

Smart Images

  • Figure 1
    Figure 1
  • Figure 2
    Figure 2
  • Figure 3
    Figure 3
Patent Text Reader

Abstract

The invention discloses a method for measuring the content of bromide ions in brine by gas chromatography. The method comprises the following steps: a. preprocessing a sample, namely, adding an acidifying agent, a derivatizing agent and an oxidizing agent into the brine in sequence, and uniformly mixing for reaction; fully reacting and adding an extracting solvent for extracting; filtering supernatant liquid by anhydrous sodium sulfate for later use; b. measuring the content, namely measuring the content of the bromide ions in the brine processed in the step a by a gas chromatograph, wherein a detector in the gas chromatograph is a hydrogen flame ionization detector. According to the method, the operation is simple, quickness is achieved, the sensitivity is high, the cost is low, the selectivity is good, the impurity interference is slight, the detection result is accurate, and the repeatability, the recovery rate and the precision are good.
Need to check novelty before this filing date? Find Prior Art

Description

technical field

[0001] The invention relates to a method for determining the content of bromide ions in brine, in particular to a method for determining the content of bromide ions in brine by gas chromatography. Background technique

[0002] my country has a vast territory, with numerous salt lakes, abundant underground brine in oil and gas fields, and seawater resources known as the treasure house of minerals. These places and resources contain a variety of rare components, such as K + 、Br - , I - , B 3+ Wait. These components have extensive and important uses in the national economy, especially bromine, which has no independent ore in nature and can only be extracted from brine so far. Bromine is rare in the earth's crust but widely distributed (its Clark value is only (5-6)10 -4 %), is a volatile liquid and is a strong dispersing element. The places with relatively high concentration of bromine in nature are underground salt brine in oil and gas fields, salt lake ...

Examples

Embodiment 1

[0101] Embodiment 1: a kind of method of gas chromatographic determination of bromide ion content in brine, comprises the following steps:

[0102] a. Sample pretreatment: Prepare a standard stock solution containing 100ppm of bromide ions with potassium bromide and deionized water; respectively take 4.0mL salt brine and put them in five 10mL stoppered test tubes with scales, add 0.00, 0.10, 0.20, 0.50, 1.00mL standard stock solutions were diluted to 5mL with deionized water; respectively, 1.0mL of 5M sulfuric acid solution, 80μL of methyl isobutyl ketone and 1.0mL of 30% hydrogen peroxide were added to 5 test tubes, and mixed evenly. React at 30°C for 1 hour; after the reaction is complete, add 2.0 mL of n-hexane to 5 test tubes for extraction; take the supernatant and pass through anhydrous sodium sulfate for later use; wherein, the preparation method of the 5M sulfuric acid solution For: take 27.8mL of 98% concentrated sulfuric acid, add water to 100mL, that is;

[0103] b...

Embodiment 2

[0106] Embodiment 2: a kind of method of gas chromatographic determination of bromide ion content in brine, comprises the following steps:

[0107] a. Sample pretreatment: prepare a standard stock solution containing 300ppm bromide ions with potassium bromide and deionized water; respectively take 4.0mL salt brine and put them in five 10mL stoppered test tubes with scales, add 0.00, 0.10, 0.20, 0.50, 1.00mL standard stock solution, dilute to 5mL with deionized water; respectively add 1.0mL hydrochloric acid solution, 80μL acetone and 1.0mL concentrated sulfuric acid to 5 test tubes, mix well, and react at 30℃ for 1h ; After the reaction is complete, add 2.0mL extraction solvent respectively in 5 test tubes to extract; take the supernatant and pass through anhydrous sodium sulfate for later use;

[0108] b. Determination of content: use a gas chromatograph to measure the solution obtained in step a according to the following chromatographic conditions: chromatographic column: 3...

Embodiment 3

[0111] Embodiment 3: a kind of method of gas chromatographic determination of bromide ion content in brine, comprises the following steps:

[0112] a. Sample pretreatment: prepare a standard stock solution containing 200 ppm of bromide ions with potassium bromide and deionized water; respectively take a volume of V liters of salt brine and place it in 5 stoppered test tubes with scales, and add in turn Different volumes of standard stock solutions were diluted to the same scale with deionized water; respectively, phosphoric acid solution, methyl ethyl ketone and nitric acid solution were added to 5 test tubes in sequence, mixed evenly, and the reaction occurred; after the reaction was complete, add extraction solvent for extraction; take the supernatant after passing through anhydrous sodium sulfate;

[0113] b. Determination of content: use a gas chromatograph to measure the solution obtained in step a according to the following chromatographic conditions: chromatographic col...