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Chloride, 8113

Chloride

DOC316.53.01017

Mercuric Thiocyanate Method (0.1 to 25.0 mg/L Cl )

Scope and Application: For water and wastewater

Method 8113

Scope and Application: For water and wastewater Method 8113 Test preparation How to use instrument-specific information

Test preparation

How to use instrument-specific information

The Instrument-specific information table displays requirements that may vary between instruments. To use this table, select an instrument then read across to find the corresponding information required to perform this test.

Table 1 Instrument-specific information

Instrument

Sample cell

Cell orientation

Adapter

DR 5000

2495402

Fill line faces user

A23618

DR 2800

2495402

Fill line faces right

DR 2700

2495402

Fill line faces right

DR/2500

2427606

DR/2400

2427606

Before starting the test:

Filter turbid samples with moderately rapid filter paper and a funnel before analysis.

Both the sample and the blank will contain mercury (D009) at a concentration regulated as a hazardous waste by the Federal RCRA. Do not pour these solutions down the drain.

Refer to the MSDS sheet for safe handling and disposal of hazardous waste. Gloves are recommended.

Collect the following items:

Description

Quantity

Ferric Ion Solution

1 mL

Mercuric Thiocyanate Solution

2 mL

Deionized Water

10 mL

Sample Cells (see Instrument-specific information)

2

Pipet, TenSette ® , 0.1 to 1.0 mL

1

Pipet tips for 0.1 to 1.0 mL TenSette pipet

2

See Consumables and replacement items for reorder information.

Chloride

Mercuric Thiocyanate method for Chloride

Stored Programs 70 Chloride Start
Stored Programs
70 Chloride
Start

1. Select the test.

Insert an adapter if required (Instrument- specific information).

Refer to the user manual for orientation.

information ). Refer to the user manual for orientation. 2. Prepared Sample: Fill a sample cell

2. Prepared Sample:

Fill a sample cell with

10 mL of sample.

2. Prepared Sample: Fill a sample cell with 10 mL of sample. 3. Blank Preparation: Fill

3. Blank Preparation:

Fill another sample cell

with 10 mL of deionized water.

Fill another sample cell with 10 mL of deionized water. 4. Pipet 0.8 mL of Mercuric

4. Pipet 0.8 mL of

Mercuric Thiocyanate Solution into each sample cell.

mL of Mercuric Thiocyanate Solution into each sample cell. 5. Swirl to mix. 9. Within five

5.

Swirl to mix.

Thiocyanate Solution into each sample cell. 5. Swirl to mix. 9. Within five minutes after the

9. Within five minutes

after the timer expires, wipe the blank and insert it into the cell holder.

expires, wipe the blank and insert it into the cell holder. 6. Ion Solution into each

6.

Ion Solution into each sample cell.

Pipet 0.4 mL of Ferric

Zero
Zero

10. ZERO the instrument.

The display will show:

0.0 mg/L Cl

the instrument. The display will show: 0.0 mg/L Cl – 7. Swirl to mix. An orange

7. Swirl to mix. An

orange color will develop if chloride is present.

to mix. An orange color will develop if chloride is present. 11. Wipe the prepared sample

11. Wipe the prepared

sample and insert it into the cell holder.

Wipe the prepared sample and insert it into the cell holder. 8. Start the instrument timer.

8. Start the instrument

timer.

A two-minute reaction time will begin.

Read
Read

12. READ the results in

mg/L Cl .

Chloride

Interferences

Table 2 Interfering substances and levels

Interfering substance

Interference levels and treatments

Extreme pH

Should be about pH 2 after adding reagents. If the sample is strongly acidic or alkaline, adjust a portion of sample before testing to a pH of about 7. Use either 5.0 N Sodium Hydroxide Standard Solution 1 or a 1:5 dilution of perchloric acid. Use pH paper; most pH electrodes will contaminate the sample with chloride.

1 See Optional reagents and apparatus.

Sample collection, preservation and storage

Collect samples in glass or plastic containers. Samples can be stored for at least 28 days at room temperature.

Accuracy check

Required for accuracy check:

Chloride Standard Solution, 1000-mg/L

50 mL mixing cylinders, three

TenSette Pipet

Standard additions method (sample spike)

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.

2. Select standard additions from the instrument menu:

Instrument

Navigate to:

DR 5000

OPTIONS>MORE>STANDARD ADDITIONS

DR 2800

OPTIONS>MORE>STANDARD ADDITIONS

DR 2700

OPTIONS>MORE>STANDARD ADDITIONS

DR/2500

OPTIONS>STANDARD ADDITIONS

DR/2400

OPTIONS>STANDARD ADDITIONS

3. Default values for standard concentration, sample volume, and spike volumes can be accepted or edited. After values are accepted, the unspiked sample reading will appear in the top row. See the user manual for more information.

4. Prepare three sample spikes. Fill three 50 mL mixing cylinders with 50 mL of sample. Use the TenSette ® Pipet to add 0.1 mL, 0.2 mL and 0.3 mL of 1000-mg/L Chloride Standard Solution, respectively, to the cylinders and mix each thoroughly.

5. Analyze a 10 mL portion of each sample spike as described in the Mercuric Thiocyanate method for Chloride test, starting with the 0.1 mL sample spike. Each addition should reflect approximately 100% recovery.

6. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard addition results to the theoretical 100% recovery.

Chloride

Standard Solution Method Required for accuracy check:

Chloride Standard Solution, 1000-mg/L

Volumetric Flask, 500-mL

Pipet, Class A glassware

1. Prepare a 20.0-mg/L chloride standard solution.

a. Use Class A glassware to pipet 10.00 mL of Chloride Standard Solution, 1000-mg/L, into a 500-mL volumetric flask.

b. Dilute to the mark with deionized water. Follow the Mercuric Thiocyanate method for Chloride test.

2. To adjust the calibration curve using the reading obtain ed with the standard solution, navigate to Standard Adjust in the software.

Instrument

Navigate to:

DR 5000

OPTIONS>MORE>STANDARD ADJUST

DR 2800

OPTIONS>MORE>STANDARD ADJUST

DR 2700

OPTIONS>MORE>STANDARD ADJUST

DR/2500

OPTIONS>STANDARD ADJUST

DR/2400

OPTIONS>STANDARD ADJUST

3. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate concentration is used, enter the concentration and adjust the curve to that value.

Method performance

Program

Instrument

Standard

 

Precision 95% Confidence Limits of Distribution

70

DR 5000

20.0

mg/L Cl

 

17.9–22.1 mg/L Cl

DR 2800

20.0

mg/L Cl

 

17.9–22.1 mg/L Cl

DR 2700

20.0

mg/L Cl

 

17.9–22.1 mg/L Cl

DR/2500

20.0

mg/L Cl

 

18.3–21.8 mg/L Cl

DR/2400

20.0

mg/L Cl

 

18.3–21.8 mg/L Cl

Program

Instrument

Standard

Portion of curve

Sensitivity Concentration change per 0.010 Abs change

70

 

DR 5000

20.0

mg/L Cl

1.0

mg/L

0.1

mg/L Cl

DR 2800

 

10.0

mg/L

   

DR 2700

0.3

mg/L Cl

 

20.0

mg/L

0.6

mg/L Cl

 

DR/2500

20.0

mg/L Cl

1.0

mg/L

0.11 mg/L Cl

DR/2400

 

20.0

mg/L

45 mg/L Cl

Chloride

Summary of method

Chloride in the sample reacts with mercuric thiocyanate to form mercuric chloride and liberate thiocyanate ion. Thiocyanate ions react with the ferric ions to form an orange ferric thiocyanate complex. The amount of this complex is proportional to the chloride concentration. Test results are measured at 455 nm.

Consumables and replacement items

Required reagents

Description

Quantity/Test

Unit

Catalog number

Chloride Reagent Set, includes:

100 tests/pkg 1

 

(1) Ferric Ion Solution

1 mL

100 mL

 

(1) Mercuric Thiocyanate Solution

2 mL

200 mL

 

Water, deionized

10 mL

4 L

1

100 tests (50 samples and 50 blanks) using 10-mL cells. 50 tests using 25-mL cells.

 

Required apparatus

 

Description

Quantity/Test

Unit

Catalog number

Pipet, TenSette ® , 0.1 to 1.0 mL

1

each

1970001

Pipet Tips, for TenSette Pipet 1970001

varies

50/pkg

2185696

Recommended standards

 

Description

 

Unit

Catalog number

Chloride Standard Solution, 1000-mg/L Cl

 

500 mL

18349

Optional reagents and apparatus

 

Description

 

Unit

Catalog number

Chloride Standard Solution, 10-mL Voluette ® Ampule, 12,500-mg/L Cl

 

16/pkg

1425010

Chloride Standard Solution, 100-mg/L

 

1 L

2370853

Cylinders, mixing

 

50 mL

189641

Filter Paper, funnel

 

100/pkg

69257

Funnel, poly

 

75 mm

108368

Gloves, chemical resistant, size 9–9.5 1

 

pair

2410104

Perchloric Acid, ACS

 

680 g

75765

pH Paper, 1.0–11.0 pH range

 

5/pkg

39133

Pipet Tips, for TenSette Pipet 1970001

 

1000/pkg

2185628

Pipet, volumetric, Class A

 

10 mL

1451538

Pipet Filler, safety bulb

 

each

1465100

Sodium Hydroxide Standard Solution, 5.0 N

 

50 mL

245026

Voluette Ampule Breaker, for 10-mL ampules

 

each

2196800

1 Other sizes available

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In the U.S.A. – Call

Outside the U.S.A. – Contact the HACH office or distributor serving you.

On the Worldwide Web –

toll-free

800-227-4224

www.hach.com

; E-mail –

techhelp@hach.com

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