CN105866324A - A method of measuring a content of citric acid or a citrate in a solution - Google Patents

A method of measuring a content of citric acid or a citrate in a solution Download PDF

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Publication number
CN105866324A
CN105866324A CN201610195545.1A CN201610195545A CN105866324A CN 105866324 A CN105866324 A CN 105866324A CN 201610195545 A CN201610195545 A CN 201610195545A CN 105866324 A CN105866324 A CN 105866324A
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China
Prior art keywords
concentration
citric acid
solution
add
sodium thiosulfate
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CN201610195545.1A
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Chinese (zh)
Inventor
和黄海
谢添
郭万根
张建军
涂凯
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China Railway Resource Group Co Ltd
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China Railway Resource Group Co Ltd
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Priority to CN201610195545.1A priority Critical patent/CN105866324A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration

Abstract

A method of measuring a content of citric acid or a citrate in a solution is provided. According to properties of a sample (with the sample being an absorption liquid sample used for producing liquid sulfur dioxide through a citric acid absorption manner), through adopting a quantitative reaction between potassium permanganate and the citric acid as a main principle, and based on a large number of practices and experiments, a rapid, accurate, economical and environmental friendly test method for the total citric acid content is summarized and provided. Detailed operation steps and a calculating manner are listed in the test method. The method is suitable for measuring the total citric acid content of the absorption liquid sample used for producing the liquid sulfur dioxide through the citric acid absorption manner. The total citric acid content of the absorption liquid sample is about 200 g/L in general. A proper amount of the sample is weighed according to practical sample content and used for detection. The proper amount of the citric acid in the sample is about 100 mg. Detection results are accurate and reliable. The accuracy of the detection results is 99% or above.

Description

Citric acid or the assay method of citrate content in a kind of solution
Technical field
The invention belongs to chemical field, particularly relate to citric acid or the mensuration of citrate content in a kind of solution Method.
Background technology
Citric acid absorption process produces in sulfur dioxide liquid technique, and it is bigger that citric acid consumption accounts for its cost ratio, And citric acid content has much relations with sulfur dioxide liquid production efficiency, quick and precisely check citric acid (salt) Content energy accurate instruction produces to be prepared rational citric acid absorbing liquid and provides strong on absorbing liquid is discarded Help.During citric acid absorption process produces sulfur dioxide liquid technique industry at present, do not find the most total lemon The standard test method of lemon acid content can depend on, and existing assay method has lead citrate gravimetric method and lead acetate to drip Determining method, lead citrate gravimetric method time-consumingly grows (detecting a sample the most time-consuming 1.5 days), and medicine used is to environment Having pollution, and method is difficult to grasp, accuracy is bad, and inspection cost is relatively high；Lead acetate titrimetry is by sample In product, the impact of sulfate and other impurity is big, and medicine used also can have the biggest pollution to environment, and titration is eventually Point is difficult to observe, and accuracy is the highest.
Summary of the invention
The problem that it is an object of the invention to exist for prior art, it is provided that citric acid (salt) in a kind of solution The assay method of content.
Above-mentioned purpose is realized by following proposal:
Citric acid or the assay method of citrate content in a kind of solution, it is characterised in that described mensuration side Method includes: pipettes 10mL sample and is placed in 100mL volumetric flask, with pure water constant volume and shake up, then pipettes 5mL Sample after pure water constant volume is placed in 400mL conical flask, adds 50mL water, adds 5mL analytical pure concentrated sulphuric acid, Heated and boiled makes sulfur dioxide all decompose (the most time-consuming 20～25min), adds water to 80mL, adds with pipet Enter the potassium permanganate solution that 20mL concentration is 0.15mol/L, in 72 DEG C of water-bath inside holding 15min, cooling To room temperature, add water to 250mL, add the KI that 10mL concentration is 200g/L, use sodium thiosulfate standard solution (the standard solution i.e. solution of 0.1mol/L) is titrated to faint yellow, adds the starch that 2mL concentration is 1g/L, Continuation sodium thiosulfate standard solution is titrated to blueness and decorporates, and record consumes sodium thiosulfate standard solution Volume V3, Unit/mL；According to the concentration of citric acid in following formula calculating solution:
H C i ( g / L ) = ( 20 - K × V 3 ) × T V s = ( 20 - K × V 3 ) × 2 × T , ( V s = 10 × 5 / 100 = 0.5 , 1 / V s = 1 / 0.5 = 2 )
In formula:
The concentration of the total citric acid of HCi (g/L), unit g/L；
K 1mL sodium thiosulfate is equivalent to the amount of potassium permanganate, Unit/mL；
T 1mL potassium permanganate is equivalent to the amount of citric acid, mg/mL
V3 titration consumes the volume of sodium thiosulfate standard solution, Unit/mL；
Vs sample volume, mL；(participate in the sample volume of titration, be 0.5mL, Vs=10 in this example × 5/100=0.5).
According to above-mentioned assay method, it is characterised in that the computational methods of K are: draw potassium permanganate solution 5mL (0.15mol/L), adds sulphuric acid that 25mL concentration is 2mol/L, adds water to 250mL, adds 10mL dense Degree is the KI of 200g/L, drips with sodium thiosulfate standard solution (the standard solution i.e. solution of 0.1mol/L) Fixed the most faint yellow, add the starch that 2mL concentration is 1g/L, (standard is molten for continuation sodium thiosulfate standard solution The liquid i.e. solution of 0.1mol/L) it is titrated to blueness and decorporates as terminal, record consumes sodium thiosulfate standard solution Volume V1, Unit/mL；Calculate
According to above-mentioned assay method, it is characterised in that the computational methods of T are: pipetting 10mL concentration is 10g/L Citric acid standard solution, add the sulphuric acid that 25mL concentration is 2mol/L, add water to 250mL, at 72 DEG C of water Heating 10min in bath, adding 20mL concentration with pipet is the potassium permanganate solution of 0.15mol/L, continues Heating in water bath 15min, is cooled to room temperature with flowing water, adds the KI that 10mL concentration is 200g/L, with sulfur for sulfur Acid sodium standard solution (the standard solution i.e. solution of 0.1mol/L) is titrated to faint yellow, and adding 2mL concentration is 1g/L Starch, continuation hypo solution is titrated to blueness and decorporates, record consume sodium thiosulfate standard molten The volume V2 of liquid；CalculateCHCiIt is the dense of citric acid standard solution Degree, this example is 10g/L.
Beneficial effects of the present invention:
This law is easily mastered (requiring operator low) in inspection, checks each process to easily determine, accuracy Good, agents useful for same relative price is the highest, and agents useful for same will not be to environment, and the time used is few, The batch detection (detection of a batch sample can be completed for about 1～2 hour) of appropriate sample.
Detailed description of the invention
In the solution of the present invention, the assay method of citric acid or citrate content includes: pipettes 10mL sample and puts In 100mL volumetric flask, with pure water constant volume and shake up, then pipette the sample after 5mL pure water constant volume and be placed in 400mL In conical flask, adding 50mL water, add 5mL analytical pure concentrated sulphuric acid, heated and boiled makes sulfur dioxide all decompose (the most time-consuming 20～25min), adds water to 80mL, and adding 20mL concentration with pipet is 0.15mol/L's Potassium permanganate solution, at 72 DEG C of water-bath inside holding 15min, is cooled to room temperature, adds water to 250mL, add 10mL concentration is the KI of 200g/L, and with sodium thiosulfate standard solution, (the i.e. 0.1mol/L's of standard solution is molten Liquid) it is titrated to faint yellow, add the starch that 2mL concentration is 1g/L, continuation sodium thiosulfate standard solution drips Determining to blueness to decorporate, record consumes the volume V3 of sodium thiosulfate standard solution, Unit/mL；According to following formula meter The concentration of citric acid in calculation solution:
H C i ( g / L ) = ( 20 - K × V 3 ) × T V s = ( 20 - K × V 3 ) × 2 × T , ( V s = 10 × 5 / 100 = 0.5 , 1 / V s = 1 / 0.5 = 2 )
In formula:
The concentration of the total citric acid of HCi (g/L), unit g/L；
K 1mL sodium thiosulfate is equivalent to the amount of potassium permanganate, Unit/mL；
T 1mL potassium permanganate is equivalent to the amount of citric acid, mg/mL
V3 titration consumes the volume of sodium thiosulfate standard solution, Unit/mL；
Vs sample volume, mL；(participate in the sample volume of titration, be 0.5mL, Vs=10 in this example × 5/100=0.5).
According to above-mentioned assay method, it is characterised in that the computational methods of K are: draw potassium permanganate solution 5mL (0.15mol/L), adds sulphuric acid that 25mL concentration is 2mol/L, adds water to 250mL, adds 10mL dense Degree is the KI of 200g/L, drips with sodium thiosulfate standard solution (the standard solution i.e. solution of 0.1mol/L) Fixed the most faint yellow, add the starch that 2mL concentration is 1g/L, (standard is molten for continuation sodium thiosulfate standard solution The liquid i.e. solution of 0.1mol/L) it is titrated to blueness and decorporates as terminal, record consumes sodium thiosulfate standard solution Volume V1, Unit/mL；Calculate
According to above-mentioned assay method, it is characterised in that the computational methods of T are: pipetting 10mL concentration is 10g/L Citric acid standard solution, add the sulphuric acid that 25mL concentration is 2mol/L, add water to 250mL, at 72 DEG C of water Heating 10min in bath, adding 20mL concentration with pipet is the potassium permanganate solution of 0.15mol/L, continues Heating in water bath 15min, is cooled to room temperature with flowing water, adds the KI that 10mL concentration is 200g/L, with sulfur for sulfur Acid sodium standard solution (the standard solution i.e. solution of 0.1mol/L) is titrated to faint yellow, and adding 2mL concentration is 1g/L Starch, continuation hypo solution is titrated to blueness and decorporates, record consume sodium thiosulfate standard molten The volume V2 of liquid；CalculateCHCi is the dense of citric acid standard solution Degree, this example is 10g/L.
Specifically describe in terms of principle, reagent and analysis method are several below.
1. assay method (principle) general introduction of the present invention
70～75 DEG C, under acid condition, potassium permanganate can carry out quantitative response with citric acid, adds in sample The Standard Potassium Permanganate Solution of excess, after residue potassium permanganate adds excess potassium iodide, measures by iodimetric titration, The interference of sulfurous acid (salt) uses and adds the removing of sulphuric acid post-heating.Chemical equation is as follows:
(3)2KMnO4+10KI+8H2SO4=2MnSO4+5I2+6KSO4+8H2O
(4)I2+2Na2S2O3=2NaI+Na2S4O6
2 main agents
2.1 sulphuric acid (2mol/L), 196.16g concentrated sulphuric acid adds in 500mL water, and cooling is settled to 1000mL；
2.2 concentrated sulphuric acids, analytical pure；
2.3 potassium iodide 200g/L, claim 100g potassium iodide to be dissolved in 500mL water；
2.4 starch indicator 1g/L, are dissolved in 100mL after weighing 1g soluble starch water furnishing pasty state In hot water, heated and boiled cooled down after about 3 minutes；
2.5 citric acid standard solution, with trisodium citrate (more than analytical pure), being configured to citric acid equivalent is 10g/L aqueous solution；
2.6 sodium thiosulfate standard solution 0.1mol/L, GB/T 601；
2.6.1 hypo solution demarcation (1mL sodium thiosulfate is equivalent to amount K of potassium permanganate, ML) draw potassium permanganate solution 5mL, add 25mL sulphuric acid (2.1), add water to 250mL, 10mL KI (2.3), It is titrated to faint yellow with sodium thiosulfate (2.6), adds 2mL starch (2.4), continue with sodium thiosulfate (2.6) It is titrated to blueness decorporate as terminal, the volume V1 (mL) of record consumption hypo solution (2.6).
K = 5 V 1
2.7 Standard Potassium Permanganate Solution 0.15mol/L, 23.7g are dissolved in 1000mL water；
2.7.1 the demarcation (1mL potassium permanganate is equivalent to amount T of citric acid, mg/mL) of potassium permanganate solution
Pipette 10mL citric acid standard solution (2.5), add 25mL sulphuric acid (2.1), add water to 250mL, In 72 DEG C of water-baths, heat 10min, add 20mL potassium permanganate solution (2.7) with pipet, continue water Bath heating 15min, is cooled to room temperature with flowing water, adds 10mL KI (2.3), use sodium thiosulfate standard solution (2.6) it is titrated to faint yellow, adds 2mL starch (2.4), continue with sodium thiosulfate standard solution (2.6) Being titrated to blueness decorporate, record consumes the volume V2 (mL) of sodium thiosulfate standard solution.
CHCiIt is citric acid standard solution (2.5) concentration, this example For 10g/L.
3 analytical procedures
3.1 pipette 10mL sample is placed in 100mL volumetric flask, with pure water constant volume and shake up, then pipettes 5mL Sample be placed in 400mL conical flask (conical flask is put into one (stirrer of magnetic stirring apparatus, about 2～ 3cm length) magnetic stirring bar), adding 50mL water, add 5mL concentrated sulphuric acid (2.2), heating makes sulfur dioxide complete Part solves (boiling 20～25min), adds water to 80mL, adds 20mL potassium permanganate solution with pipet (2.7), at 72 DEG C of water-bath inside holding 15min, it is cooled to room temperature with flowing water, adds water to 250mL, add 10mL KI (2.3), is titrated to faint yellow with sodium thiosulfate standard solution (2.6), adds 2mL starch (2.4), Continuation hypo solution (2.6) is titrated to blueness and decorporates, and it is molten that record consumes sodium thiosulfate standard The volume V3 (mL) of liquid (2.6).
H C i ( g / L ) = ( 20 - K × V 3 ) × T V s = ( 20 - K × V 3 ) × 2 × T , ( V s = 10 × 5 / 100 = 0.5 , 1 / V s = 1 / 0.5 = 2 )
In formula:
The concentration of the total citric acid of HCi (g/L), unit g/L；
K 1mL sodium thiosulfate is equivalent to the amount of potassium permanganate, Unit/mL；
T 1mL potassium permanganate is equivalent to the amount of citric acid, mg/mL
V3 titration consumes the volume of sodium thiosulfate standard solution, Unit/mL；
Vs sample volume, mL；(participate in the sample volume of titration, be 0.5mL, Vs=10 in this example × 5/100=0.5).

Claims (3)

  1. null1. citric acid or the assay method of citrate content in a solution，It is characterized in that，Described assay method includes: pipettes 10mL sample and is placed in 100mL volumetric flask，With pure water constant volume and shake up，Pipette 5mL sample again to be placed in 400mL conical flask，Add 50mL water，Add 5mL analytical pure concentrated sulphuric acid，Heated and boiled makes sulfur dioxide all decompose，Add water to 80mL，Adding 20mL concentration with pipet is the potassium permanganate solution of 0.15mol/L，At 72 DEG C of water-bath inside holding 15min，It is cooled to room temperature，Add water to 250mL，Add the KI that 10mL concentration is 200g/L，It is titrated to faint yellow with the sodium thiosulfate standard solution that concentration is 0.1mol/L，Add the starch that 2mL concentration is 1g/L，Continuation sodium thiosulfate standard solution is titrated to blueness and decorporates，Record consumes the volume V3 of sodium thiosulfate standard solution，Unit/mL；According to the concentration of citric acid in following formula calculating solution:
    In formula:
    The concentration of the total citric acid of HCi (g/L), unit g/L；
    K 1mL sodium thiosulfate is equivalent to the amount of potassium permanganate, Unit/mL；
    T 1mL potassium permanganate is equivalent to the amount of citric acid, mg/mL
    V3 titration consumes the volume of sodium thiosulfate standard solution, Unit/mL；
    Vs sample volume, mL.
  2. Assay method the most according to claim 1, it is characterized in that, the computational methods of K are: draw the potassium permanganate solution 5mL of 0.15mol/L, adding sulphuric acid that 25mL concentration is 2mol/L, add water to 250mL, adding 10mL concentration is the KI of 200g/L, is titrated to faint yellow with sodium thiosulfate standard solution, add the starch that 2mL concentration is 1g/L, continuation sodium thiosulfate standard solution is titrated to blueness and decorporates as terminal, the volume V1 of record consumption sodium thiosulfate standard solution, Unit/mL；Calculate
  3. Assay method the most according to claim 1, it is characterized in that, the computational methods of T are: pipette the citric acid standard solution that 10mL concentration is 10g/L, add the sulphuric acid that 25mL concentration is 2mol/L, add water to 250mL, 10min is heated in 72 DEG C of water-baths, adding 20mL concentration with pipet is the potassium permanganate solution of 0.15mol/L, continue heating in water bath 15min, it is cooled to room temperature with flowing water, add the KI that 10mL concentration is 200g/L, it is titrated to faint yellow with sodium thiosulfate standard solution, add the starch that 2mL concentration is 1g/L, continuation hypo solution is titrated to blueness and decorporates, record consumes the volume V2 of sodium thiosulfate standard solution；CalculateCHCiIt is the concentration of citric acid standard solution.
CN201610195545.1A 2016-03-31 2016-03-31 A method of measuring a content of citric acid or a citrate in a solution Pending CN105866324A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112611749A (en) * 2020-10-30 2021-04-06 重庆金美新材料科技有限公司 Method for detecting content of ammonium citrate in liquid

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
冯开文: "中性镀镍溶液柠檬酸钠的测定", 《电镀与精饰》 *
劳光启: "镍钨非晶镀液中柠檬酸的氧化还原测定", 《上海钢研》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112611749A (en) * 2020-10-30 2021-04-06 重庆金美新材料科技有限公司 Method for detecting content of ammonium citrate in liquid

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Application publication date: 20160817