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GB/T 11896-1989 PDF English

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GB/T 11896-1989: [GB 11896-1989] Water quality. Determination of chloride. Silver nitrate titration method
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GB/T 11896-1989: [GB 11896-1989] Water quality. Determination of chloride. Silver nitrate titration method


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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA GB/T 11896-1989 Water Quality – Determination of Chloride – Silver Nitrate Titration Method APPROVED ON. DECEMBER 25, 1989 Implemented on. JULY 01, 1990 Approved by. State Bureau of Environmental Protection

Table of Contents

1 Theme Content and Applicable Range... 3 2 Principle... 3 3 Reagents... 3 4 Instruments... 5 5 Sample... 5 6 Analytical Procedures... 5 7 Result Expression... 6 8 Precision and Accuracy... 6 Appendix A Determination of the Highly Mineralized Salt Water and Seawater (Supplement)... 8 Additional Instructions... 9 Water Quality – Determination of Chloride – Silver Nitrate Titration Method

1 Theme Content and Applicable Range

This Standard specifies using the silver nitrate titration method to determine the concentration of chloride in water. This Standard is applicable to the determination of chloride in the natural water; it is also applicable to the highly mineralized water that has been diluted, such as salt water, seawater, etc.; as well as applicable to the domestic sewage and industrial wastewater that has removed the interference through the pretreatment. This Standard is applicable to the chloride with concentration of 10~500mg/L. The water sample above such range can expand its determination range after dilution. The bromide, iodide and cyanide can be titrated together with chloride. When the orthophosphate and polyphosphate separately exceed 250mg/L and 25mg/L, they have interference. When iron content exceeds 10 mg/L, the end-point is not obvious.

2 Principle

In the neutral or weak alkaline range (pH 6.5~10.5), take potassium chromate as an indicator; when using silver nitrate to titrate the chloride, since the solubility of silver chloride is less than that of the silver chromate, chloride ion is firstly precipitated fully; then the chromate was precipitated in the form of silver chromate; generate brick red, which indicates that the titration end-point is reached. The titration reaction of the precipitation is as follows.

3 Reagents

Only use analytical reagent to prepare during the analyzing period; as well as distilled water or deionized water. Brick red 3.1 Potassium permanganate, C (1/5 KMnO4) =0.01mol/L. 3.2 Hydrogen peroxide (H2O2), 30%. 3.3 Ethanol (C6H5OH), 95%. 3.4 Sulfuric acid solution, C (1/2 H2SO4) = 0.05mol/L. 3.5 Sodium hydroxide solution, C (NaOH) = 0.05mol/L. 3.6 Aluminum hydroxide suspension. dissolve 125g of potassium aluminum sulfate [KAl (SO4)2 • 12H2O] into 1L of distilled water; heating to 60°C; then slowly add 55mL of stronger ammonia water as stir, stand for about 1h; then move to larger bottle; use pouring method to repeatedly wash the precipitant till the eluate doesn’t contain the chloride ions. Use water to dilute to about 300mL. 3.9 Potassium chromate solution, 50g/L. take 5g of potassium chromate (K2CrO4); dissolve into little amount of distilled water; titrate silver nitrate solution (3.8) till red precipitant is generated. Shake evenly, stand for 12h; then filter it, and use distilled water to dilute the filtrate to 100mL. 3.10 Phenolphthalein indicator solution. take 0.5g of phenolphthalein; dissolve into 50mL of 95% ethanol (3.3). Add 50mL of distilled water; then titrate 0.05mol/L sodium hydroxide solution (3.5), so that the slight red appears.

4 Instruments

4.1 Conical flask, 250mL. 4.2 Burette, 25mL, brown.

5 Sample

Take representative water sample, place into the clean and chemically stable glass or polyethylene bottle. When storing, it is not necessary to add anti-corrosive agent.

6 Analytical Procedures

6.1 Interference exclusion If there aren’t various interferences below, such section can be omitted. 6.1.1 If the water sample is turbid and has a color, then take 150mL or appropriate amount of water sample to dilute to 150mL; then place into 250mL conical flask; add 2mL of aluminum hydroxide suspension (3.6); shake and filter; discard the 20mL of initial filtrate; then use clean conical flask to receive filtrate for spare-use. 6.2 Determination 6.2.1 Pipette 50mL of water sample or pre-treated water sample (if the chloride content is high, take appropriate amount of water sample, dilute with distilled water to 50mL); then place into conical flask. Take another conical flask; add 50mL of distilled water to take blank test. 6.2.2 If water sample’s pH value is in the range of 6.5~10.5, it can be titrated directly; the water sample beyond such range shall take phenolphthalein as indicator; use dilute sulfur acid (3.4) or sodium hydroxide solution (3.5) to adjust till the red just appears.

7 Result Expression

The chloride content C (mg/L) shall be calculated as follows.

8 Precision and Accuracy

The results of 6-laboratory determination against the standard mixed sample containing 88.29mg/L of chloride (January 1987) are as follows. 8.1 Repeatability The relative standard deviation in the laboratory is 0.27%. 8.2 Reproducibility The relative standard deviation between the laboratories is 1.2%.

Appendix A

Determination of the Highly Mineralized Salt Water and Seawater (Supplement) A.1 For the determination of the highly mineralized salt water and seawater, the following methods can be taken to expand its determination range1). a. Improve the concentration of silver nitrate standard solution to the 2~5mg of chloride equivalent to 1mL of standard solution. b. Dilute the sample; the dilution factor can refer to Table 1. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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