HACH Cloruros

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Chloride

Page 1 of 6

Chloride, 8113

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.

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

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) 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.

http://doc316.53.01000.pdf/

http://doc316.53.01000.pdf/

http://doc316.53.01000.pdf/



Chloride

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Chloride

Mercuric Thiocyanate method for Chloride

1. Select the test.

Insert an adapter if

required (Instrument-

specific information).

Refer to the user manual

for orientation.

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 .

5. Swirl to mix. 6. Pipet 0.4 mL of Ferric

Ion Solution into eachsample cell. Not e: Use 0.5

mL with DR 5000 .

7. Swirl to mix. An

orange color will develop ifchloride is present.

8. Start the instrument

timer. A two-minute reaction time

will begin.

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 –

11. Wipe the prepared

sample and insert it into

the cell holder.

12. READ the results in

mg/L Cl –.

70 Chloride

Stored Programs

Start

Zero Read



Chloride

Chloride

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Interferences

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.

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.

1 See Optional reagents and apparatus.



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

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 thiocyanatecomplex. The amount of this complex is proportional to the chloride concentration. Test results are

measured at 455 nm.

Consumables and replacement items

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 – 17.9–22.1 mg/L Cl – 0.1 mg/L Cl – 1.0 mg/L

0.3 mg/L Cl – 10.0 mg/L

0.6 mg/L Cl – 20.0 mg/L

Required reagents

Description Quantity/Test Unit Catalog number

Chloride Reagent Set, includes: — 250 tests/pkg1

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

2319800

(1) Ferric Ion Solution 1 mL 100 mL 2212242

(1) Mercuric Thiocyanate Solution 2 mL 200 mL 2212129

Water, deionized 10 mL 4 L 27256

Required apparatus

Description Quantity Unit Catalog number

Pipet, TenSette®, 0.1 to 1.0 mL 1 each 1970001

Pipet Tips, for TenSette Pipet 1970001 varies 50/pkg 2185696

Sample cell, 10 mL square, matched pair 2 2/pkg 2495402

Recommended standards

Description Unit Catalog number

Chloride Standard Solution, 1000-mg/L Cl – 500 mL 18349

http://www.hach.com/hc/search.product.details.invoker/PackagingCode=2319800










Chloride

Chloride

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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 Cl – 1 L 2370853

Cylinder, mixing, 50 mL each 189641

Filter Paper, funnel, 125 mm 100/pkg 69257

Funnel, poly, 75 mm each 108368

Gloves, chemical resistant, size 9–9.51

1 Other sizes available

pair 2410104

Perchloric Acid, ACS 680 g 75765

pH Paper, 1.0–11.0 pH range, 15 foot roll 5/pkg 39133

Pipet Tips, for TenSette Pipet 1970001 1000/pkg 2185628

Pipet, volumetric, Class A, 10 mL each 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



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HACH Cloruros