206-98166

HYDRIDE VAPOR GENERATOR

for Shimadzu Atomic Absorption Spectrophotometer

HVG-1

Service Manual
 206-98166

Contents

1. Introduction ........................................................................................................................................... 2
2. Installation Procedure .......................................................................................................................... 4
3. Checking Performance and Acceptance Conditions ........................................................................... 5
4. Adjustment Procedure .......................................................................................................................... 7
5. Measurement Principle ........................................................................................................................ 9
6. Preparing Reagents ............................................................................................................................ 10
7. Troubleshooting................................................................................................................................... 12
8. HVG-1 (P/N 206-17143-4x/5x) Parts list
 HVG-1 Service Manual

1. Introduction

1.1 Product Overview

The HVG-1 hydride vapor generator is used in combination with Shimadzu atomic absorption
spectrophotometers (AA-7000 series, AA-6200, AA-6300, or AA-6800/6650 series models) to quantify
the concentration of arsenic (As), selenium (Se), antimony (Sb), mercury (Hg), or other elements in
sample solutions, based on the hydride generation method.

1.2 Notice
The prescribed service training is required to use this service manual properly. Therefore, please
understand that Shimadzu cannot be responsible for any problems that may result from using this
service manual without the proper training.

1.3 Warning Labels

The following warning labels are used on HVG-1 units. These labels are affixed in the locations indicated
in the yellow pages of the instruction manual.

(1) Warning label: Corrosion warning (Part No.: 037-72138-00)

Warning message: This container contains corrosive chemicals. Do not touch or spill its contents.
(2) Warning label: Exhaust and handling warning (Part No.: 206-58756)

Warning message:  This product generates hydrogen or metal hydride gases during operation. Be
sure to operate an exhaust duct.
 Be sure to read the instruction manual regarding how to handle waste liquids
properly.

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1.4 Safety Precautions

(1) Locations that receive power even when the power switch is OFF (power supply voltage)
Wires between the AC power inlet and the power switch
Disconnect the instrument from the power supply before touching these areas.
Be especially careful to prevent any conductive personal accessories (such as rings and necklaces)
from touching high voltage areas.

(2) Locations that receive power even when the power switch is OFF
All wiring
Wear insulating gloves before touching inside the instrument when connected to power.
Be especially careful to prevent any conductive personal accessories (such as rings and necklaces)
from touching high voltage areas.

(3) Water inside tubing/pipes

Remove all liquids, such as liquids inside flow lines and samples, before performing maintenance with
the cover open. Spilling any of these liquids could cause short circuits.

(4) Confirming safety after service work

After switching the power ON, use an electrical tester to confirm that there is no voltage to ground (both
AC and DC) from metallic surfaces on the exterior.

1.5 Precautions During Installation

(1) Screw tips
When lifting the product, be careful to avoid injury from screw tips protruding from the bottom.

(2) Power cord

Use the power cord provided with the instrument.

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 HVG-1 Service Manual

2. Installation Procedure
HVG-1 units are thoroughly inspected at the plant before shipping. To ensure optimal performance and
customer satisfaction, install the instrument according to the following procedure.

2.1 Confirming Installation Site Requirements

Before installing the HVG-1, refer to the installation requirements and 9.4 Environmental Requirements
in the instruction manual to make sure the installation site is appropriate. Install the main HVG-1 unit as
close to the absorption cell as possible. The fluorinated rubber tubing for connecting to the absorption
cell is 1 m long. Install the HVG-1 unit within an area that can be reached with that tubing. The main unit
weighs about 10 kg. Using an inappropriate posture to lift the unit could cause injury. Using a commercial
cart with caster wheels to move the instrument is recommended.

2.2 Verifying Standard Accessories

To avoid unwanted problems, refer to 1.2 Details of Parts in the instruction manual to verify, together with
the user, that all standard accessory parts are present.

2.3 Installation
Refer to 3.1 Installation Procedure in the instruction manual to install the HVG-1 unit.
If installing it at the same time as a GFA unit, install the argon gas lines using the three-way nipple splitter
assembly provided.

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 HVG-1 Service Manual

3. Checking Performance and Acceptance Conditions

3.1 Supplies Required for Checking Performance

(1) Graduated cylinder (10 mL) 1
(2) Stopwatch 1
(3) Reagents
 Sodium borohydride solution (0.4 % NaBH4 + 0.5 % NaOH) 500 mL
 Hydrochloric acid (5 M HCl) 500 mL
(4) Sample
 Standard As solution (10 ppb) 500 mL
(5) Distilled water
 Prepare the sodium borohydride and standard As solution immediately prior to measurements.
Sensitivity decreases with time.
 For instructions on preparing reagents, see 6. Preparing Reagents and refer to 4. Reagent
Preparation and Sample Pretreatment in the instruction manual.

3.2 Maximum Pump Flowrate

Refer to 4.1 Reagent Preparation in the instruction manual to rotate the pump and set the speed control
knob to the maximum setting. Confirm the following flowrates by using the pump to aspirate distilled
water from the graduated cylinder. However, measure the flowrate after the pump has warmed up for
about ten minutes.
(1) Reagent: Minimum 2.8 mL/min with 60 Hz power or minimum 2.5 mL/min with 50 Hz power (for
NaBH4 and HCl)
(2) Sample: Minimum 8.0 mL/min with 60 Hz power or minimum 7.0 mL/min with 50 Hz power

3.3 Confirming the Flush Function

(1) Set the speed control knob approximately in the center and press the [FLUSH] switch.
(2) Confirm that the flush indicator light illuminates, the rotor rotates at maximum flowrate speed for
about 20 to 25 seconds, and then the rotor returns to its previous speed before the flush switch was
pressed.

3.4 Confirming the Pressure Switch Function

(1) Confirm that the [PRESSURE] indicator light illuminates and the pump rotor stops when the gas
supply pressure is reduced to 0.28  0.2 MPa or lower. (The [PRESSURE] indicator light rotor stops.)
(2) Confirm that the [PRESSURE] indicator light switches OFF and the pump rotor starts rotating when
the gas supply pressure is increased to 0.28  0.2 MPa or higher.
(3) After confirming the pressure switch, adjust the gas supply pressure to 0.35MPa.

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 HVG-1 Service Manual

3.5 Confirming the Sensitivity and C.V. Values

(1) Connect the HVG-1 hydride vapor generator to the atomic absorption spectrophotometer and
measure the 10 ppb As solution five times with the following conditions.
 Sample: As 10 ppb
 Reagent: 5 M HCl acid
 Reagent: 0.4 % NaBH4 + 0.5 % NaOH solution reducing agent
 Flame: C2H2 2.0 mL/min
 Sample flowrate: 5.5 mL/min
 Integration time: 10 sec
 Repeats: 5 times
(2) Confirm that sensitivity and C.V. values are as indicated below.
 Sensitivity: Min. 0.25 Abs
 C.V.: Max. 5 %

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 HVG-1 Service Manual

4. Adjustment Procedure

4.1 Supplies Required for Adjustment

 Flow meter assembly (775-07217) 1
 0.5 MPa pressure gauge (200-93553-02) 1
 Ar gas
 Stopwatch 1
 10 mL graduated cylinder 1
 Reagents
Sodium borohydride solution (0.4 % NaBH4 + 0.5 % NaOH) 500 mL
Hydrochloric acid (5 M HCl) 500 mL
 Sample: As (10 ppb) 500 mL
 Distilled water

4.2 Adjusting the Flow Lines

4.2.1 Adjusting the Ar Gas Flowrate (Gas Supply)

圧力計
Pressure gauge 流量計
Flow meter

NV1

圧力SW
Pressure switch
Solenoid
電磁弁
valve NV2
Ar

0.35MPa Pressure
調圧器
regulator

206-17112-41 イリグチポ-ト
206-17112-41 クミタテ
Inlet Port ASSY

Fig. 1 Ar Gas Flowrate System

(1) Install the pressure gauge (0.5 MPa) in an open port on the pressure regulator.
(2) Supply 0.35 MPa Ar gas.
(3) Switch the main unit ON.
(4) Set the needle valve (NV1 and 2) knobs to roughly the center position (about four turns from fully
closed).
(5) Turn the pressure regulator knob to adjust pressure to 0.25 MPa.
(6) Connect the flow meter to needle valve NV1 and turn the knob to adjust the flowrate to
32.5  1 mL/min. Read the flowrate level at the center of the float.
(7) Similarly, connect the flow meter to needle valve NV2 and turn the knob to adjust the flowrate to
32.5  1 mL/min.

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 HVG-1 Service Manual

(8) Confirm that the pressure gauge indicates 0.25  0.01 MPa. If it has shifted, repeat steps (5) to (7).
(9) Disconnect the flow meter.

4.2.2 Confirming the Pressure Switch Function

(1) Gradually decrease the Ar gas supply pressure from 0.35 MPa and read the pressure where the
[PRESSURE] indicator light switches ON and the pump motor stops rotating.
Specifications: 0.26 to 0.30 MPa
(2) Next, gradually increase the Ar gas supply pressure and read the pressure where the [PRESSURE]
indicator light switches OFF and the pump motor starts rotating.
Specifications: 0.26 to 0.30 MPa
(3) Set the Ar gas supply pressure to 0.35 MPa.
(4) Confirm that the pressure gauge indicates 0.25 MPa. If it has shifted, reset the pressure using the
pressure regulator.
(5) Disconnect the Ar gas supply line.
(6) Disconnect the pressure gauge and install the plug (hex screw). Be sure to apply pipe sealant to the
threads.
(7) Switch the main unit OFF.

4.2.3 Setting the Flush Timer

Turn the timer dial to 22.5 seconds. (Somewhere between 22 and 23 is OK.)
Press the flush button and use a stopwatch to measure how long the flush function remains active to
confirm that it functions for between 20 and 25 seconds.

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 HVG-1 Service Manual

5. Measurement Principle

The aqueous As, Se, Sb, or other solution reacts with hydrogen in the generator to produce gaseous
hydrides. These hydrides are sent to the atomization unit where they are atomized by thermal
dissociation to enable high-sensitivity analysis.
In the presence of the reducing agent, the inorganic mercury (Hg) in the aqueous solution is vaporized
as liberated mercury. By sending this vapor to the atomic absorption unit, atomic absorption can be
measured without heating.
The pump sends the respective sample and reagent (hydrochloric acid and sodium borohydride)
solutions to the manifold, where they are mixed. Then the mixture is sent to the reaction coil, where it
forms hydrides.
Carrier gas carries these hydrides, and any hydrogen, water vapor, and residual reagent liquids
generated at the same time, to the gas-liquid separator. The separator separates the gas phase from the
liquid phase and drains the liquid phase, so that the carrier gas carries only the gas phase to the
absorption cell. Then the absorption cell is heated with an air-acetylene flame to atomize the target
measurement elements, by dissociating the hydrides, and measure their atomic absorption. The mercury,
however, is analyzed in the same cell, but without heating.

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 HVG-1 Service Manual

6. Preparing Reagents

For instructions on preparing reagents, refer to 4. Reagent Preparation and Sample Pretreatment in the
instruction manual.

6.1 Equipment Required for Preparing Reagents (assuming 500 mL is prepared of each)
(1) Pipette 1 mL 1
(2) Pipette 5 mL 1
(3) Pipette 10 mL 1
(4) Volumetric flask 100 mL 2
(5) Volumetric flask 500 mL 1
(6) Graduated cylinder 500 mL 1
(7) Beaker 100 mL 2
(8) Rubber pipetter bulb 1
(9) Digital balance 1
(10) Plastic tank 500 mL 4
(More may be needed depending on the quantities prepared.)

6.2 Purchased Reagents

(1) Sodium borohydride (NaBH4)
(2) Sodium hydroxide (NaOH)
(3) Hydrochloric acid (HCl)
(4) Arsenic (As) 1000 ppm
(5) Distilled water
Analytical grade (25 g bottle)
Analytical grade (500 g bottle)
Analytical grade (500 mL bottle)
Standard solution for atomic absorption

6.3 Reagents and Quantities Required (to be Prepared) for Adjustment and Inspection
(1) NaBH4 (0.4 % NaBH4 + 0.5 % NaOH solution) 100 mL (per unit)
(2) 5 M HCl 100 mL (per unit)
(3) 10 ppb As 100 mL (per unit)
Note 1: Includes quantities for inspections using two absorption cells included as accessories.
Note 2: 50 mL of the 10 ppb As is sufficient for one absorption cell.

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 HVG-1 Service Manual

6.4 Preparing Reagents

6.4.1 Standard As Solution (10 ppb)
(1) Using the 1 mL pipette, take 1 mL from the 1000 ppm standard As solution and place it in a 100 mL
volumetric flask. Add distilled water to make 100 mL.  10 ppm
(2) Using the 10 mL pipette, take 10 mL from the sample prepared in (1) and place it in a 100 mL
volumetric flask. Add additional distilled water to make 100 mL.  1 ppm = 1000 ppb
(3) 10 ppb As solution (for preparing 500 mL)
Using the 5 mL pipette, take 5 mL from the sample prepared in (2) and place it in a 500 mL volumetric
flask. Add distilled water to make 500 mL.  10 ppb

6.4.2 NaBH4 and HCl

For instructions on preparing NaBH4 and HCl reagents, refer to 4. Reagent Preparation and Sample
Pretreatment in the instruction manual.

6.4.3 Precautions for Using Reagents

(1) Wear protective gloves and eyewear when handling reagents.
(2) Prepare reagents immediately before adjustment and inspection.
(3) Reagent preparations can be used for two days, but store them in the refrigerator.
(4) Never touch sodium hydroxide (NaOH) with bare hands. (Doing so will cause burns.)
(5) Do not leave the sodium hydroxide bottle cap off. (It is highly deliquescent.)
(6) If any of the reagents contact hands or other areas, immediately rinse the area with tap water.
(7) Be sure to switch ON the exhaust system during inspection.
(8) To dispose of sodium borohydride, place it in a separate disposal container without mixing it with
other waste liquids.

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7. Troubleshooting
Symptoms
Power will not switch ON.
Rotor does not turn.
Flush function does not function.
Sensitivity is low.
Reproducibility is poor.
HVG-1 Service Manual
Causes
Blown fuse
Speed controller knob is set to
lowest setting.
The supply pressure dropped.
(The [PRESSURE] indicator light
is illuminated.)
The timer has failed.
Timer time setting
The timer has failed.
The flush switch has failed.
HCl current value is low.
The HCl has deteriorated.
The optical axis is not hitting the
absorption cell.
The reagent has deteriorated.
The absorption cell has
deteriorated.
Insufficient reagent and/or
sample flowrate
HCl current value is low.
The HCl has deteriorated.
The optical axis is not hitting the
absorption cell.
Pump tubing has deteriorated.
The manifold has clogged.
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Corrective Measures
Replace the fuse.
Turn the knob.
Set the gas supply pressure to
0.35 MPa.
Replace the timer.
Reset the timer.
Replace the timer.
Replace the flush switch.
Set the current to an appropriate
value.
Replace the indicator light.
Adjust the absorption cell
position.
Replace the reagent with new
reagent.
Replace the absorption cell with
a new one.
 Increase the pump rpm.
 Replace the pump tubing.
 Check for leaks in the flow
lines.
 If the pump tubing is pinched
anywhere, loosen it (particularly
at clamps).
 Adjust the pressure regulator
and needle valves.
Set the current to an appropriate
value.
Replace the indicator light.
Adjust the absorption cell
position.
Replace the pump tubing.
Clean or replace the manifold.
 HVG-1 Service Manual
Motor rotation is not smooth.
Tubing is leaking.
The pressure regulator is not
functioning properly.
A needle valve is defective.
13
Replace the motor and motor
controller.
Replace any deteriorating tubing
and joints.
Replace the pressure regulator.
Replace the needle valve.
 HVG-1 Service manual

8. HVG-1 (P/N 206-17143-4x/5x) Parts list

FRONT SIDE
14 17 18 22 4 20，21 1，2 13

9，10，11

19 15，16 12 5 6 7 8

1 206-17123 PRESSING PLATE For Sample Tube

2 206-17124 PRESSING PLATE For NaBH4, HCl tube
3 206-17118 Roller ASSY
4 072-60319 Cramp,DKN-13SP
5 206-58758-41 FLASH SW ASSY
6 206-58759-41 INDICATOR LIGHT ASSY,PRESSURE
7 206-58759-42 INDICATOR LIGHT ASSY,FLASH
8 064-14543-12 SWITCH,ROCKER A8L-21-15N3
9 206-17127 Screw
10 034-01056-01 SPRING,C221
11 206-17126 PIN,HVG-1
12 037-30059-07 DAMPER,TM-96-07
13 206-18067 SCREW CATCH ASSY
14 206-58755 CAP,ADD.WORK
15 204-09363-02 BOTTLE, ADD. WORK
16 037-72143-00 LABEL,CAUTION SA40-143P
037-72138-00 LABEL,CAUTION SA40-138P
17 206-18036-02 TUBE ASSY,HCL
18 206-18036-01 TUBE ASSY, NaBH4
 HVG-1 Service manual

19 206-18036-03 TUBE ASSY,SAMPLE

20 208-90038-08 PUMP TUBING,08 For NaBH4,HCl
21 208-90038-13 PUMP TUBING,13 For SAMPLE
22 206-17879-01 SIDE COVER
 HVG-1 Service manual

LEFT SIDE

15

11

10

7，8

14

13

12

5 1 2，3，4 6 16

1 206-18032 TRAY ASSY

2 206-60250-03 TUBE Vinyl 1
3 204-64601 HOSE Nipple
4 200-62522 O RING,EPR
5 206-60250-04 TUBE VINYL 2
6 206-18033 GUIDE PLATE
7 206-58790-41 INLET ASSY
8 072-02004-11 FUSE,218.315P
072-02004-16 FUSE,218 001.P
9 206-17839 VAPOR SEPARATOR
10 036-12504 O-RING,4D G40
 HVG-1 Service manual

11 206-18037 REACTION COIL ASSY

12 206-17825 MANIFORD
13 206-60250-02 TUBE DRAIN
14 072-60315-01 WIRING CLAMP,RF100
15 206-58756 LABEL,HVG
206-58757 LABEL,HVG E
16 206-18069-41 FRONT COVER ASSY
 HVG-1 Service manual

TOP VIEW (COVER OPENED)

1 2 3 6

7 5 4 8

1 032-53739-61 GEAR HEAD,2GB30K-D2

2 200-84586-03 MOTOR,CONTROL 2IJ3RGB-A-E2
3 206-58784-41 CAP ASSY
4 066-19469-02 TIMER,PM4HA-H-AC240VW
5 206-17114 NEEDLE VALVE ASSY
6 077-89432-01 CONTROLLER,ES01
7 206-17112-41 INLET PORT ASSY
8 208-95844-01 TRANSFORMER,HVG
 HVG-1 Service manual

RIGHT SIDE (COVER OPENED)

1 206-17113 VALVE ASSY

2 040-72532 REGULATOR,B2019-1CP
3 206-58700-42 PRESSURE SWITCH ASSY
4 035-60617 COUPLER,22PMT
 HVG-1 Service manual

ELECTRIC CIRCUIT DIAGRAM

 HVG-1 Service manual

MOTOR CONTROLLER

Terminal S4 and S6
 HVG-1 Service manual

FLOW PATH DIAGRAM