Chloride, 8113

How to use Tinin

Chloride DOC316.53.01017Mercuric Thiocyanate Method Method 8113(0.1 to 25.0 mg/L Cl)Scope and Application: For water and wastewater

Test prep

Instrument

DR 6000

DR 5000

DR 3900

DR 3800, DR 280

Before starting t

Filter turbid sampl

Both the sample aRCRA. Do not pou

Refer to the MSDS

Collect the follow

Description

Ferric Ion Solution

Mercuric Thiocyan

Deionized Water

Sample Cells (see

Pipet, TenSette,

Pipet tips for 0.1 to

See ConsumablesChloridePage 1 of 6

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

aration

Table 81 Instrument-specific information

Sample cell Cell orientation

2495402 Fill line faces right

2495402 Fill line faces user

2495402 Fill line faces user

0, DR 2700 2495402 Fill line faces right

he test:

es with moderately rapid filter paper and a funnel before analysis.

nd the blank will contain mercury (D009) at a concentration regulated as a hazardous waste by the Federal r these solutions down the drain.

sheet for safe handling and disposal of hazardous waste. Gloves are recommended.

ing items:

Quantity

1 mL

ate Solution 2 mL

10 mL

Instrument-specific information) 2

0.1 to 1.0 mL 1

1.0 mL TenSette pipet 2

and replacement items for reorder information.

ChloridePage 2 of 6

Chloride

Mercuric Thiocyanate method for Chloride

1. Select the tesInsert an adapter required (Instrumespecific informatioRefer to the user for orientation.

5. Swirl to mix.

9. Within five miafter the timer expwipe the blank andinto the cell holde

70 Chloride

Stored Programs

Startt.if nt-n).

manual

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.A two-minute reaction time will begin.

nutes ires, insert it

r.

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.

Zero Read

Chloride

Interferences

Sample collCte

Accuracy chR

S

1

2

3

4

5

6

SR

1

Table 82 Interfering substances and levelsInterfering 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

1 See Optional reagenChloridePage 3 of 6

ection, preservation and storageollect samples in glass or plastic containers. Samples can be stored for at least 28 days at room mperature.

eckequired for accuracy check:

Chloride Standard Solution, 1000-mg/L

50 mL mixing cylinders (3)

TenSette Pipet and tips

tandard additions method (sample spike)

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

. Select Options>More>Standard additions from the instrument menu.

. 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.

. 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.

. 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.

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

tandard Solution Methodequired for accuracy check:

Chloride Standard Solution, 1000-mg/L

Volumetric Flask, 500-mL

Pipet, Class A, 10 mL

. 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.

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.

ts and apparatus.

ChloridePage 4 of 6

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 ofCthcm

Consumable

Program

70 2

Required reagen

Description

Chloride Reagent S

1 This test requires a

(1) Ferric Ion S

(1) Mercuric T

Water, deionized

Required appara

Description

Pipet, TenSette, 0

Pipet Tips, for TenS

Sample cell, 10 mL

Recommended s

Description

Chloride Standard methodhloride in the sample reacts with mercuric thiocyanate to form mercuric chloride and liberate iocyanate ion. Thiocyanate ions react with the ferric ions to form an orange ferric thiocyanate

omplex. The amount of this complex is proportional to the chloride concentration. Test results are easured at 455 nm.

s and replacement items

StandardPrecision

95% Confidence Limits of Distribution

SensitivityConcentration changeper 0.010 Abs change

Portion of curve

0.0 mg/L Cl 17.922.1 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

ts

Quantity/Test Unit Catalog number

et, includes: 250 tests/pkg1

reagent blank. The number of tests shown refers to any combination of samples and blanks.

2319800

olution 1 mL 100 mL 2212242

hiocyanate Solution 2 mL 200 mL 2212129

10 mL 4 L 27256

tus

Quantity Unit Catalog number

.1 to 1.0 mL 1 each 1970001

ette Pipet 1970001 varies 50/pkg 2185696

square, matched pair 2 2/pkg 2495402

tandards

Unit Catalog number

Solution, 1000-mg/L Cl 500 mL 18349

Chloride

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, 5

Filter Paper, funne

Funnel, poly, 75 m

Gloves, chemical r

1 Other sizes availabl

Perchloric Acid, AC

pH Paper, 1.011.0

Pipet Tips, for TenS

Pipet, volumetric, C

Pipet Filler, safety

Sodium Hydroxide

Voluette Ampule BChloridePage 5 of 6

0 mL each 189641

l, 125 mm 100/pkg 69257

m each 108368

esistant, size 99.51

e

pair 2410104

S 680 g 75765

pH range, 15 foot roll 5/pkg 39133

ette Pipet 1970001 1000/pkg 2185628

lass A, 10 mL each 1451538

bulb each 1465100

Standard Solution, 5.0 N 50 mL 245026

reaker, for 10-mL ampules each 2196800

Hach Company, 2HACH COMPANYWORLD HEADQUARTERSTelephone: (970) 669-3050FAX: (970) 669-2932

FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:Call 800-227-4224

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007, 2010, 2012. All rights reserved. Printed in the U.S.A. Edition 7

ChlorideMercuric Thiocyanate MethodMethod 8113(0.1 to 25.0 mg/L Cl)