Chloride, 8113

Chloride

DOC316.53.01017

Mercuric Thiocyanate Method

(0.1 to 25.0 mg/L

Method 8113

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 81 Instrument-specific information

Instrument

Sample cell

Cell orientation

DR 6000

2495402

Fill line faces right

DR 5000

2495402

Fill line faces user

DR 3900

2495402

Fill line faces user

DR 3800, DR 2800, DR 2700

2495402

Fill line faces right

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)

Pipet, TenSette, 0.1 to 1.0 mL

Pipet tips for 0.1 to 1.0 mL TenSette pipet

See Consumables and replacement items for reorder information.

Chloride
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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. Note: Use 1.0 mL
with DR 5000.

6. Pipet 0.4 mL of Ferric

Ion Solution into each
sample cell. Note: Use 0.5
mL with DR 5000.

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.

Chloride
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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 82 Interfering substances and levels

Interfering substance

Interference levels and treatments

Extreme pH

The pH should be about 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 (3)

TenSette Pipet and tips

Standard additions method (sample spike)

1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
2. Select Options>More>Standard additions from the instrument menu.
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.
Standard Solution Method
Required for accuracy check:

Chloride Standard Solution, 1000-mg/L

Volumetric Flask, 500-mL

Pipet, Class A, 10 mL

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

a. 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.

Chloride
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Chloride
2. To adjust the calibration curve using the reading obtained with the standard solution, select
Options>More>Standard Adjust from the instrument menu.
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

Standard

Precision
95% Confidence Limits of
Distribution

Sensitivity
Concentration change
per 0.010 Abs change

Portion of curve

70

20.0 mg/L Cl

17.922.1 mg/L Cl

0.1 mg/L Cl

1.0 mg/L

Cl

10.0 mg/L

0.6 mg/L Cl

20.0 mg/L

0.3 mg/L

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:

250 tests/pkg1

2319800

(1) Ferric Ion Solution

1 mL

100 mL

2212242

(1) Mercuric Thiocyanate Solution

2 mL

200 mL

2212129

10 mL

4L

27256

Water, deionized
1

This test requires a reagent blank. The number of tests shown refers to any combination of samples and blanks.

Required apparatus
Description
Pipet,

TenSette,

Quantity
0.1 to 1.0 mL

Pipet Tips, for TenSette Pipet 1970001

Sample cell, 10 mL square, matched pair

Unit

Catalog number
1970001

each

varies

50/pkg

2185696

2/pkg

2495402

Unit

Catalog number

500 mL

18349

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

Chloride
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Chloride

Optional reagents and apparatus

Description
Chloride Standard Solution, 10-mL Voluette Ampule, 12,500-mg/L Cl
Chloride Standard Solution, 100-mg/L Cl
Cylinder, mixing, 50 mL
Filter Paper, funnel, 125 mm
Funnel, poly, 75 mm

Catalog number

16/pkg

1425010

1L

2370853

each

189641

100/pkg

69257

each

108368

pair

2410104

Perchloric Acid, ACS

680 g

75765

pH Paper, 1.011.0 pH range, 15 foot roll

5/pkg

39133

1000/pkg

2185628

Pipet, volumetric, Class A, 10 mL

each

1451538

Pipet Filler, safety bulb

each

1465100

Gloves, chemical resistant, size 99.51

Pipet Tips, for TenSette Pipet 1970001

Sodium Hydroxide Standard Solution, 5.0 N

Voluette Ampule Breaker, for 10-mL ampules
1

Unit

50 mL

245026

each

2196800

Other sizes available

Chloride
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Edition 7