TIANJIN CHENGYI INTERNATIONAL

TRADING CO.,LIMITED
Room 1309, Wufeng Building, No.11 Zhenxing Street,
National Hi-Tech Industrial Development Zone of Taiyuan, Shanxi, China.
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EDTA 2NA ANALYSIS METHOD

Specification:

GRADE Guarantee Reagent Analytical Chemically

Purity 99.5%min 99.0%min 98.0%min

pH 4.0-5.0 4.0-5.0 4.0-5.0

Chloride (cl) 0.004%max 0.005%max 0.02%max

Sulfate (SO4) 0.01%max 0.02%max 0.1%max

C6H9NO6(NTA) 0.05%max

Fe 0.0005%max 0.001%max 0.005%max

Cu 0.00025%max

Heavy Metal(as Pb) 0.001%max 0.001max 0.005max

1 Determination of Content of Ethylene Diamine Tetraacetic Acid (EDTA) Series

1.1 Methodology

Dissolved samples into water, after which using complexometry to determine the content of
EDTA 2NA in the solution by calculating the consumption of zinc chloride standard solution,
eriochrome black T is used as indicator.

1.2 Reagents and Materials

1.2.1 Ammonia-Ammonium chloride buffer solution A (PH=10) Weighting 54g ammonia chloride,
dilute it to 1000ml after adding 360ml aqueous ammonia.

1.2.2 Zinc chloride standard titration solution: C(ZnCl2) is about 0.1 mol/L
 TIANJIN CHENGYI INTERNATIONAL
TRADING CO.,LIMITED
Room 1309, Wufeng Building, No.11 Zhenxing Street,
National Hi-Tech Industrial Development Zone of Taiyuan, Shanxi, China.
Tel: +86 351 8281246 8281248 Fax:+86 351 8206170 Email:info@tjcyint.com

1.2.3 5g/L Eriochrome black T

Weighing 0.5g eriochrome black T and 2g hydroxylamine hydrochloride, grind it in a mortar and dilute
it to 100ml.

1.3 Analysis Procedures

Dissolving 1g sample with an accuracy of 0.0001g by 100mL hot water and 10ml ammonia-ammonium
chloride buffer solution A, 5 drops of Eriochrome black T are added as indicator. Titrating the solution
by Zinc chloride standard solution until the last drop which makes the solution changes from blue to
magenta.

1.4 Results

The mass fraction (X, %) of EDTA 2NA is calculated by the follow equation.

Where,

V---Consumption of Zinc chloride standard titration solution, ml

c--- Exact concentration of Zinc chloride standard titration solution, mol/l

372.2- The molar mass of EDTA 2NA ,g/mol

m---Mass of sample, g

2 Determination of pH

2.1 Methodology

The pH value of EDTA is tested by acidimeter which equipped with glass electrode and saturated
calomel electrode (or combination electrode).

2.2 Reagents Water without CO2

2.3 Apparatus

Acidimeter with unit of 0.02pH

2.4 Analysis procedures

Weighting appropriate amount of sample, dilute it to 5% or 1% aqueous solution by water without CO2.
Determine the pH of solution by acidimeter.

The result is obtained by calculating the arithmetic mean value of Parallel determination results, the
absolute value of the Parallel determination results shall not be over 0.2pH.

3 Appearance of solution

Weighting 5g sample, dissolved it into 100ml warm water, the turbidity shall not be over than that
stipulated in HG/T—1168-1978:

Guarantee Reagent (GR), Analytical Reagent (AR)---------number 3

Chemically Pure (CP)--------------------------------------------number 5

4 Determination of Chloride (Cl)

4.1 Preparation of solution A

Weighting 2.0g sample into 25ml water and dissolving it by heating. After cooling the solution, filter it
and dilute the filtrate to 100ml.

4.2 Determination

Transfer 2ml 25% salpeter solution and 1ml 17g/l silver nitrate solution into 10ml solution A. Diluting
the solution to 25ml and shake up. Keep it for 10mins and the turbidity of the solution shall not be over
than standard turbidimetric solution.

The standard turbidimetric solution is prepared by dilution of Chloride standard solution which contains
0.02mg Cl. The solution is diluted to 10ml and treated by the same method as solution A.

5 Determination of Sulfate (SO4)

Transfer 0.5ml 20% hydrochloric acid and 3ml 25% barium chloride solution into 10ml solution A.
Diluting the solution to 25ml and shake up. Keep it for 10mins and the turbidity of the solution shall not
be over than standard turbidimetric solution.
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TRADING CO.,LIMITED
Room 1309, Wufeng Building, No.11 Zhenxing Street,
National Hi-Tech Industrial Development Zone of Taiyuan, Shanxi, China.
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The standard turbidimetric solution is prepared by dilution of sulfate standard solution which contains
0.10mg SO4. The solution is diluted to 10ml and treated by the same method as solution A.

6 Determination of NTA

6.1 NTA standard solution [1mL solution containing 1 mg am nta(C6H9NO6)]

Weigh 1.00g NTA, add 50mL water, add sodium hydroxide solution (200g/L) dropwise under shaking,
dissolve it, and dilute it to 1000ml.

6. 2 instrument conditions

Instrument: pulse or oscilloscope;

Working electrode: drop mercury electrode;

Reference electrode: Ag/AgCl or saturated calomel electrode;

Counter electrode: Platinum electrode.

Sensitivity: Appropriate choice (control of 5mg NTA generated wave height of not less than 5 mm);

Oxygen method: the nitrogen over 5 min;

Scanning potential: -0. 6 V~-1.1V;

Complex of aminotriacetic acid and pot Potential of electrolysis: About -0.9V

6.3 Determination method

Weigh 2g sample, add 30mL hot water dissolved, cooled, with sodium hydroxide solution (100g / L) to
adjust the solution pH value of 10.5~10.7

(With acidometer control), the dropwise addition of tin chloride solution (50 g / L) to the solution until
a small amount of precipitation apppear (the solution should be maintained at a pH of 10.5~10.7), add
sodium hydroxide solution(0.02g/L) ,dilute it to 100ml. Take 50 mL, measured by polarography, and its
wave height shall not be greater than half of the standard solution of the wave height.

Standard comparison solution is to take the remaining 50ml test solution and containing 0.5g NTA
standard solution, measured by polarography.
 TIANJIN CHENGYI INTERNATIONAL
TRADING CO.,LIMITED
Room 1309, Wufeng Building, No.11 Zhenxing Street,
National Hi-Tech Industrial Development Zone of Taiyuan, Shanxi, China.
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7 Determination of Fe (Atomic Absorption Method)

The standard solution is prepared by using 1000ug/ml stock solution (supported by National Nonferrous
Metals and Electronic Materials Testing Center). Transfer 1.00ml standard solution, dilute with
deionized water to 100ml. The concentration of the diluted solution is 10ug/ml. Transfer 0.5, 2.0, 5.0 ml
solution separately and dilute them with deionized water to 50ml, thus the concentration of them are 0.1,
0.4, 1.0 ug/ml respectively.

Weighting 1.0g sample with an accuracy of 0.1mg, dissolve it by deionized water to 50ml. The
deionized water is used as reference blank solution. Determine the Fe in sample solution by drawing the
standard curves.

The content of Fe in EDTA 2NA is calculated by the following equation:

Where

M---Content of Fe in sample, mg/kg

C---Content of Fe in solution which is obtained from the standard curves, ug/ml

V---Volume of diluted sample, ml

m---Mass of sample, g

8 Determination of Cu

Take 10 mL of the test solution , add 5 mL of citric acid solution (200 g/L), and adjust the pH of the
solution to 9 with aqueous ammonia and excess1 m L, diluted to 25 mL, add 1 mL sodium
diethyldithiocarbamate solution (1 g/L), shake, add 5 mL isoamyl alcohol extraction. The organic layer
is yellow shall not be deeper than the standard solution.

Preparation of standard comparison solution is copper (Cu) standard solution (containing 0.0025mg
Cu),dilut it to 10 mL and treated identically with the same volume of test solution.
 TIANJIN CHENGYI INTERNATIONAL
TRADING CO.,LIMITED
Room 1309, Wufeng Building, No.11 Zhenxing Street,
National Hi-Tech Industrial Development Zone of Taiyuan, Shanxi, China.
Tel: +86 351 8281246 8281248 Fax:+86 351 8206170 Email:info@tjcyint.com

9 Determination of Heavy Metals (Pb): Atomic Absorption Method

The standard solution is prepared by using 1000ug/ml stock solution (supported by National Nonferrous
Metals and Electronic Materials Testing Center). Transfer 1.00ml standard solution, dilute with
deionized water to 100ml. The concentration of the diluted solution is 10ug/ml. Transfer 0.5, 2.0, 5.0 ml
solution separately and dilute them with deionized water to 50ml, thus the concentration of them are 0.1,
0.4, 1.0 ug/ml respectively.

Weighting 1.0g sample with an accuracy of 0.1mg, dissolve it by deionized water to 50ml. The
deionized water is used as reference blank solution. Determine the Pb in sample solution by drawing the
standard curves.

The content of Pb in EDTA 2NA is calculated by the following equation:

Where

M---Content of Pb in sample, mg/kg

C---Content of Pb in solution which is obtained from the standard curves, ug/ml

V---Volume of diluted sample, ml

m---Mass of sample, g