Chloride 8113

Chloride, 8113

Chloride

DOC316.53.01017

Mercuric Thiocyanate Method

Method 8113

(0.1 to 25.0 mg/L Cl–) Scope and Application: For water and wastewater

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 Page 1 of 6

Chloride Mercuric Thiocyanate method for Chloride

Stored Programs 70 Chloride Start

1. Select the test. Insert an adapter if required (Instrumentspecific information).

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

3. Blank Preparation: Fill another sample cell with 10 mL of deionized water.

4. Pipet 0.8 mL of Mercuric Thiocyanate Solution into each sample cell.

6. Pipet 0.4 mL of Ferric Ion Solution into each sample cell.

7. Swirl to mix. An orange color will develop if chloride is present.

8. Start the instrument timer.

Refer to the user manual for orientation.

5. Swirl to mix.

Zero

9. Within five minutes after the timer expires, wipe the blank and insert it into the cell holder.


10. ZERO the instrument. The display will show: 0.0 mg/L Cl–

A two-minute reaction time will begin.

Read

11. Wipe the prepared sample and insert it into the cell holder.

12. READ the results in mg/L Cl–.

Chloride

Interferences Table 2 Interfering substances and levels

1

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 Solution1 or a 1:5 dilution of perchloric acid. Use pH paper; most pH electrodes will contaminate the sample with chloride.

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


DR 2700


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 obtained with the standard solution, navigate to Standard Adjust in the software. Instrument

Navigate to:

DR 5000

OPTIONS>MORE>STANDARD ADJUST

DR 2800


DR 2700


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 DR 2800 DR 2700

20.0 mg/L Cl–

1.0 mg/L

0.1 mg/L Cl–

10.0 mg/L

0.3 mg/L Cl–

20.0 mg/L

0.6 mg/L Cl–

1.0 mg/L

0.11 mg/L Cl–

20.0 mg/L

45 mg/L Cl–

DR/2500 DR/2400


20.0 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

—

100 tests/pkg1

2319800

Chloride Reagent Set, includes:

1

(1) Ferric Ion Solution

1 mL

100 mL

2212242

(1) Mercuric Thiocyanate Solution

2 mL

200 mL

2212129

Water, deionized

10 mL

4L

27256

Quantity/Test

Unit

Catalog number

1

each

1970001

varies

50/pkg

2185696

Unit

Catalog number

500 mL

18349

Unit

Catalog number

16/pkg

1425010

1L

2370853

50 mL

189641

100/pkg

69257

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

Required apparatus Description Pipet, TenSette®, 0.1 to 1.0 mL Pipet Tips, for TenSette Pipet 1970001

Recommended standards Description Chloride Standard Solution, 1000-mg/L Cl–

Optional reagents and apparatus Description Chloride Standard Solution, 10-mL Voluette® Ampule, 12,500-mg/L Cl– Chloride Standard Solution, 100-mg/L Cylinders, mixing Filter Paper, funnel Funnel, poly

75 mm

108368

pair

2410104

Perchloric Acid, ACS

680 g

75765

pH Paper, 1.0–11.0 pH range

5/pkg

39133

1000/pkg

2185628

10 mL

1451538

each

1465100

50 mL

245026

each

2196800

Gloves, chemical resistant, size

9–9.51

Pipet Tips, for TenSette Pipet 1970001 Pipet, volumetric, Class A Pipet Filler, safety bulb Sodium Hydroxide Standard Solution, 5.0 N Voluette Ampule Breaker, for 10-mL ampules 1

Other sizes available


FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: In the U.S.A. – Call toll-free 800-227-4224 Outside the U.S.A. – Contact the HACH office or distributor serving you. On the Worldwide Web – www.hach.com; E-mail – [email protected]

© Hach Company, 2007. All rights reserved. Printed in the U.S.A.

HACH COMPANY WORLD HEADQUARTERS Telephone: (970) 669-3050 FAX: (970) 669-2932

Updated February 2008, Edition 5

Chloride 8113

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